# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers # This journal is © The Partner Organisations 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a #TrackingRef 'web_deposit_cif_file_0_Taoxie_1364731106.A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H72 O12' _chemical_formula_weight 1153.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 17.548(4) _cell_length_b 24.274(5) _cell_length_c 14.468(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6163(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13994 _cell_measurement_theta_min 1.1604 _cell_measurement_theta_max 27.4644 _exptl_crystal_description rod _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3098 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007HF + CCD (Saturn724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36553 _diffrn_reflns_av_R_equivalents 0.0863 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5417 _reflns_number_gt 5082 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1486P)^2^+11.8273P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5417 _refine_ls_number_parameters 414 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.1395 _refine_ls_R_factor_gt 0.1251 _refine_ls_wR_factor_ref 0.3503 _refine_ls_wR_factor_gt 0.3265 _refine_ls_goodness_of_fit_ref 1.336 _refine_ls_restrained_S_all 1.335 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.0310(2) 0.26440(15) 0.7297(2) 0.0388(9) Uani 1 1 d . . . O2 O 0.1511(2) 0.39276(14) 0.7711(2) 0.0364(9) Uani 1 1 d . . . O3 O 0.3604(2) 0.51983(16) 0.6885(3) 0.0479(10) Uani 1 1 d . . . O4 O 0.6052(2) 0.45016(16) 0.5989(3) 0.0460(10) Uani 1 1 d . . . O5 O 0.8057(3) 0.1855(3) 0.4453(5) 0.098(2) Uani 1 1 d . . . C1 C -0.1025(4) 0.2891(3) 0.7495(4) 0.0517(15) Uani 1 1 d . . . H1A H -0.1434 0.2672 0.7215 0.078 Uiso 1 1 calc R . . H1B H -0.1037 0.3265 0.7240 0.078 Uiso 1 1 calc R . . H1C H -0.1099 0.2907 0.8166 0.078 Uiso 1 1 calc R . . C2 C -0.0152(3) 0.2617(2) 0.6354(3) 0.0318(11) Uani 1 1 d . . . C3 C -0.0269(3) 0.2124(2) 0.5880(4) 0.0337(11) Uani 1 1 d . . . C4 C -0.0086(3) 0.2113(2) 0.4943(4) 0.0410(13) Uani 1 1 d . . . H4 H -0.0158 0.1779 0.4611 0.049 Uiso 1 1 calc R . . C5 C 0.0199(3) 0.2570(2) 0.4470(4) 0.0384(12) Uani 1 1 d . . . H5 H 0.0315 0.2550 0.3830 0.046 Uiso 1 1 calc R . . C6 C 0.0309(3) 0.3055(2) 0.4963(4) 0.0329(11) Uani 1 1 d . . . C7 C 0.0132(3) 0.30803(19) 0.5904(3) 0.0302(11) Uani 1 1 d . . . C8 C 0.0275(3) 0.36460(19) 0.6329(3) 0.0312(11) Uani 1 1 d . . . H8 H 0.0147 0.3663 0.7002 0.037 Uiso 1 1 calc R . . C9 C -0.0188(3) 0.40506(19) 0.5746(4) 0.0328(11) Uani 1 1 d . . . C10 C -0.0747(3) 0.4406(2) 0.6077(5) 0.0439(14) Uani 1 1 d . . . H10 H -0.0866 0.4423 0.6717 0.053 Uiso 1 1 calc R . . C11 C -0.1128(3) 0.4736(2) 0.5435(5) 0.0473(14) Uani 1 1 d . . . H11 H -0.1522 0.4975 0.5640 0.057 Uiso 1 1 calc R . . C12 C -0.0945(3) 0.4722(2) 0.4527(5) 0.0535(17) Uani 1 1 d . . . H12 H -0.1204 0.4960 0.4111 0.064 Uiso 1 1 calc R . . C13 C -0.0384(3) 0.4365(2) 0.4183(4) 0.0452(14) Uani 1 1 d . . . H13 H -0.0261 0.4359 0.3544 0.054 Uiso 1 1 calc R . . C14 C -0.0016(3) 0.4023(2) 0.4805(4) 0.0326(11) Uani 1 1 d . . . C15 C 0.0606(3) 0.3602(2) 0.4579(3) 0.0326(11) Uani 1 1 d . . . H15 H 0.0731 0.3584 0.3905 0.039 Uiso 1 1 calc R . . C16 C 0.1298(3) 0.37602(19) 0.5186(3) 0.0306(11) Uani 1 1 d . . . C17 C 0.1118(3) 0.37746(18) 0.6130(3) 0.0279(10) Uani 1 1 d . . . C18 C 0.1681(3) 0.38946(18) 0.6772(3) 0.0278(10) Uani 1 1 d . . . C19 C 0.2426(3) 0.40111(19) 0.6486(3) 0.0301(11) Uani 1 1 d . . . C20 C 0.2585(3) 0.4004(2) 0.5539(3) 0.0330(11) Uani 1 1 d . . . H20 H 0.3087 0.4085 0.5334 0.040 Uiso 1 1 calc R . . C21 C 0.2026(3) 0.3881(2) 0.4893(3) 0.0332(11) Uani 1 1 d . . . H21 H 0.2145 0.3880 0.4253 0.040 Uiso 1 1 calc R . . C22 C 0.1438(3) 0.3407(2) 0.8168(4) 0.0448(14) Uani 1 1 d . . . H22A H 0.1054 0.3184 0.7850 0.067 Uiso 1 1 calc R . . H22C H 0.1281 0.3466 0.8810 0.067 Uiso 1 1 calc R . . H22B H 0.1930 0.3215 0.8156 0.067 Uiso 1 1 calc R . . C23 C 0.3024(3) 0.4116(2) 0.7225(4) 0.0372(12) Uani 1 1 d . . . H23B H 0.2861 0.4438 0.7595 0.045 Uiso 1 1 calc R . . H23A H 0.3035 0.3794 0.7645 0.045 Uiso 1 1 calc R . . C24 C 0.3824(3) 0.4219(2) 0.6884(3) 0.0328(11) Uani 1 1 d . . . C25 C 0.4078(3) 0.4751(2) 0.6707(3) 0.0318(11) Uani 1 1 d . . . C26 C 0.4829(3) 0.4857(2) 0.6405(4) 0.0377(12) Uani 1 1 d . . . C27 C 0.5312(3) 0.4405(2) 0.6298(3) 0.0332(11) Uani 1 1 d . . . C28 C 0.5079(3) 0.3862(2) 0.6456(4) 0.0330(11) Uani 1 1 d . . . C29 C 0.4327(3) 0.3788(2) 0.6752(4) 0.0348(11) Uani 1 1 d . . . H29 H 0.4154 0.3423 0.6868 0.042 Uiso 1 1 calc R . . C30 C 0.3151(4) 0.5386(3) 0.6123(5) 0.0565(17) Uani 1 1 d . . . H30B H 0.3466 0.5400 0.5564 0.085 Uiso 1 1 calc R . . H30C H 0.2953 0.5755 0.6258 0.085 Uiso 1 1 calc R . . H30A H 0.2725 0.5132 0.6025 0.085 Uiso 1 1 calc R . . C31 C 0.5090(4) 0.5434(2) 0.6199(4) 0.0470(14) Uani 1 1 d . . . H31A H 0.4653 0.5657 0.6002 0.071 Uiso 1 1 calc R . . H31B H 0.5471 0.5426 0.5704 0.071 Uiso 1 1 calc R . . H31C H 0.5315 0.5596 0.6756 0.071 Uiso 1 1 calc R . . C32 C 0.6596(3) 0.4584(3) 0.6700(5) 0.0589(17) Uani 1 1 d . . . H32B H 0.7097 0.4654 0.6424 0.088 Uiso 1 1 calc R . . H32A H 0.6622 0.4254 0.7090 0.088 Uiso 1 1 calc R . . H32C H 0.6445 0.4901 0.7078 0.088 Uiso 1 1 calc R . . C33 C 0.5613(3) 0.3379(2) 0.6321(4) 0.0437(13) Uani 1 1 d . . . H33A H 0.6047 0.3503 0.5935 0.052 Uiso 1 1 calc R . . H33B H 0.5821 0.3273 0.6931 0.052 Uiso 1 1 calc R . . C34 C 0.7010(7) 0.1789(5) 0.5415(9) 0.124(4) Uani 1 1 d . . . H34B H 0.6602 0.2065 0.5425 0.185 Uiso 1 1 calc R . . H34C H 0.7389 0.1879 0.5888 0.185 Uiso 1 1 calc R . . H34A H 0.6795 0.1424 0.5542 0.185 Uiso 1 1 calc R . . C35 C 0.7370(4) 0.1787(3) 0.4511(6) 0.068(2) Uani 1 1 d . . . C36 C 0.6891(6) 0.1709(4) 0.3704(8) 0.109(4) Uani 1 1 d . . . H36A H 0.6636 0.1351 0.3743 0.164 Uiso 1 1 calc R . . H36C H 0.7205 0.1723 0.3145 0.164 Uiso 1 1 calc R . . H36B H 0.6507 0.2002 0.3680 0.164 Uiso 1 1 calc R . . O6 O 0.3091(8) 0.2636(6) 0.6512(11) 0.094(3) Uani 0.522(12) 1 d PDU A 1 C37 C 0.3048(10) 0.2644(7) 0.5516(12) 0.090(4) Uani 0.522(12) 1 d PDU A 1 O6A O 0.3033(7) 0.2742(5) 0.7180(10) 0.087(3) Uani 0.478(12) 1 d PDU . 2 C37A C 0.2656(13) 0.2593(10) 0.6359(12) 0.089(4) Uani 0.478(12) 1 d PDU . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.044(2) 0.041(2) 0.0314(19) 0.0061(15) 0.0012(15) 0.0008(16) O2 0.043(2) 0.041(2) 0.0252(18) -0.0050(15) 0.0047(15) -0.0007(15) O3 0.059(2) 0.044(2) 0.041(2) -0.0071(17) -0.0031(18) 0.0172(19) O4 0.0346(19) 0.045(2) 0.058(3) -0.0016(19) 0.0047(18) -0.0100(16) O5 0.070(4) 0.119(5) 0.106(5) -0.005(4) 0.020(3) -0.016(3) C1 0.059(4) 0.059(4) 0.037(3) -0.005(3) 0.009(3) 0.000(3) C2 0.030(2) 0.036(3) 0.030(3) 0.003(2) -0.0045(19) 0.004(2) C3 0.029(2) 0.028(2) 0.043(3) 0.000(2) -0.005(2) 0.0002(19) C4 0.038(3) 0.032(3) 0.053(3) -0.009(2) -0.005(2) 0.000(2) C5 0.040(3) 0.045(3) 0.030(3) -0.009(2) -0.001(2) 0.006(2) C6 0.029(2) 0.033(3) 0.037(3) 0.000(2) -0.004(2) 0.0026(19) C7 0.031(2) 0.030(2) 0.029(3) 0.003(2) 0.002(2) 0.0033(19) C8 0.037(3) 0.029(2) 0.028(3) -0.004(2) 0.000(2) 0.000(2) C9 0.033(3) 0.025(2) 0.040(3) 0.000(2) -0.001(2) -0.0045(19) C10 0.031(3) 0.037(3) 0.064(4) -0.003(3) -0.004(2) -0.003(2) C11 0.036(3) 0.035(3) 0.071(4) 0.003(3) -0.005(3) 0.003(2) C12 0.043(3) 0.039(3) 0.079(5) 0.020(3) -0.020(3) -0.002(3) C13 0.043(3) 0.036(3) 0.056(4) 0.014(3) -0.017(3) -0.002(2) C14 0.032(3) 0.029(2) 0.037(3) 0.003(2) -0.004(2) -0.0009(19) C15 0.037(3) 0.039(3) 0.023(2) 0.002(2) -0.005(2) 0.001(2) C16 0.036(3) 0.026(2) 0.030(3) 0.006(2) -0.006(2) 0.0094(19) C17 0.035(2) 0.024(2) 0.025(2) 0.0014(19) 0.0023(19) 0.0067(19) C18 0.037(2) 0.023(2) 0.023(2) 0.0016(18) -0.0009(19) 0.0079(19) C19 0.035(2) 0.026(2) 0.029(3) 0.0012(19) 0.000(2) 0.0088(19) C20 0.032(2) 0.035(3) 0.032(3) 0.001(2) 0.003(2) 0.005(2) C21 0.041(3) 0.038(3) 0.021(2) 0.007(2) 0.002(2) 0.007(2) C22 0.053(3) 0.050(3) 0.032(3) 0.006(2) -0.005(2) -0.009(3) C23 0.034(3) 0.047(3) 0.031(3) -0.004(2) 0.005(2) 0.004(2) C24 0.033(3) 0.044(3) 0.021(2) -0.002(2) -0.006(2) 0.005(2) C25 0.038(3) 0.030(2) 0.027(3) -0.008(2) -0.003(2) 0.007(2) C26 0.050(3) 0.033(3) 0.030(3) -0.004(2) -0.006(2) -0.009(2) C27 0.032(2) 0.039(3) 0.029(3) -0.004(2) -0.002(2) -0.003(2) C28 0.031(2) 0.031(3) 0.037(3) -0.004(2) -0.001(2) -0.001(2) C29 0.036(3) 0.031(3) 0.037(3) 0.003(2) -0.001(2) -0.004(2) C30 0.064(4) 0.050(4) 0.055(4) -0.006(3) -0.016(3) 0.019(3) C31 0.058(3) 0.029(3) 0.055(4) -0.002(2) -0.004(3) -0.004(2) C32 0.036(3) 0.059(4) 0.081(5) 0.001(3) -0.004(3) -0.010(3) C33 0.036(3) 0.038(3) 0.057(4) 0.001(3) 0.006(3) 0.003(2) C34 0.102(8) 0.125(9) 0.143(10) 0.001(8) 0.054(7) -0.010(7) C35 0.048(4) 0.056(4) 0.099(6) -0.003(4) 0.014(4) -0.001(3) C36 0.119(8) 0.077(6) 0.132(9) 0.006(6) -0.053(7) 0.015(5) O6 0.093(5) 0.073(5) 0.116(6) 0.012(5) -0.007(5) 0.005(5) C37 0.086(6) 0.074(6) 0.108(6) 0.004(6) 0.006(6) 0.008(5) O6A 0.088(5) 0.070(5) 0.102(6) 0.011(5) 0.000(5) 0.010(4) C37A 0.086(6) 0.071(6) 0.111(6) 0.007(5) -0.003(6) 0.011(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.394(6) . ? O1 C1 1.421(7) . ? O2 C18 1.393(6) . ? O2 C22 1.431(6) . ? O3 C25 1.392(6) . ? O3 C30 1.433(7) . ? O4 C27 1.393(6) . ? O4 C32 1.419(7) . ? O5 C35 1.219(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.391(7) . ? C2 C3 1.395(7) . ? C3 C4 1.394(8) . ? C3 C33 1.504(7) 2 ? C4 C5 1.397(8) . ? C4 H4 0.9500 . ? C5 C6 1.389(7) . ? C5 H5 0.9500 . ? C6 C7 1.399(7) . ? C6 C15 1.530(7) . ? C7 C8 1.525(7) . ? C8 C9 1.528(7) . ? C8 C17 1.538(7) . ? C8 H8 1.0000 . ? C9 C10 1.392(7) . ? C9 C14 1.397(7) . ? C10 C11 1.397(8) . ? C10 H10 0.9500 . ? C11 C12 1.353(9) . ? C11 H11 0.9500 . ? C12 C13 1.402(9) . ? C12 H12 0.9500 . ? C13 C14 1.384(7) . ? C13 H13 0.9500 . ? C14 C15 1.532(7) . ? C15 C16 1.547(7) . ? C15 H15 1.0000 . ? C16 C21 1.377(7) . ? C16 C17 1.403(7) . ? C17 C18 1.387(7) . ? C18 C19 1.400(7) . ? C19 C20 1.398(7) . ? C19 C23 1.519(7) . ? C20 C21 1.388(7) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22C 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.509(7) . ? C23 H23B 0.9900 . ? C23 H23A 0.9900 . ? C24 C29 1.382(7) . ? C24 C25 1.391(7) . ? C25 C26 1.412(7) . ? C26 C27 1.395(7) . ? C26 C31 1.503(7) . ? C27 C28 1.399(7) . ? C28 C29 1.400(7) . ? C28 C33 1.513(7) . ? C29 H29 0.9500 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C30 H30A 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32B 0.9800 . ? C32 H32A 0.9800 . ? C32 H32C 0.9800 . ? C33 C3 1.504(7) 2 ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.453(13) . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C34 H34A 0.9800 . ? C35 C36 1.451(12) . ? C36 H36A 0.9800 . ? C36 H36C 0.9800 . ? C36 H36B 0.9800 . ? O6 C37 1.443(16) . ? O6A C37A 1.406(17) . ? O6A C37A 1.88(2) 2 ? C37A C37A 0.71(4) 2 ? C37A O6A 1.88(2) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 O1 C1 113.1(4) . . ? C18 O2 C22 114.7(4) . . ? C25 O3 C30 115.9(4) . . ? C27 O4 C32 114.8(4) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 O1 119.4(4) . . ? C7 C2 C3 121.1(5) . . ? O1 C2 C3 119.5(4) . . ? C4 C3 C2 117.4(5) . . ? C4 C3 C33 119.3(5) . 2 ? C2 C3 C33 123.2(5) . 2 ? C3 C4 C5 122.9(5) . . ? C3 C4 H4 118.5 . . ? C5 C4 H4 118.5 . . ? C6 C5 C4 118.2(5) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? C5 C6 C7 120.4(5) . . ? C5 C6 C15 126.6(5) . . ? C7 C6 C15 113.0(4) . . ? C2 C7 C6 119.9(4) . . ? C2 C7 C8 126.8(4) . . ? C6 C7 C8 113.3(4) . . ? C7 C8 C9 105.6(4) . . ? C7 C8 C17 105.4(4) . . ? C9 C8 C17 106.1(4) . . ? C7 C8 H8 113.0 . . ? C9 C8 H8 113.0 . . ? C17 C8 H8 113.0 . . ? C10 C9 C14 121.1(5) . . ? C10 C9 C8 125.7(5) . . ? C14 C9 C8 113.2(4) . . ? C9 C10 C11 117.7(6) . . ? C9 C10 H10 121.2 . . ? C11 C10 H10 121.2 . . ? C12 C11 C10 121.2(6) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 121.8(5) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C14 C13 C12 117.9(6) . . ? C14 C13 H13 121.1 . . ? C12 C13 H13 121.1 . . ? C13 C14 C9 120.3(5) . . ? C13 C14 C15 126.5(5) . . ? C9 C14 C15 113.1(4) . . ? C6 C15 C14 105.0(4) . . ? C6 C15 C16 106.1(4) . . ? C14 C15 C16 105.8(4) . . ? C6 C15 H15 113.1 . . ? C14 C15 H15 113.1 . . ? C16 C15 H15 113.1 . . ? C21 C16 C17 120.2(4) . . ? C21 C16 C15 127.3(5) . . ? C17 C16 C15 112.5(4) . . ? C18 C17 C16 119.8(4) . . ? C18 C17 C8 127.0(4) . . ? C16 C17 C8 113.2(4) . . ? C17 C18 O2 120.8(4) . . ? C17 C18 C19 120.6(4) . . ? O2 C18 C19 118.5(4) . . ? C20 C19 C18 118.3(4) . . ? C20 C19 C23 123.6(4) . . ? C18 C19 C23 118.1(4) . . ? C21 C20 C19 121.4(5) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C16 C21 C20 119.6(5) . . ? C16 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? O2 C22 H22A 109.5 . . ? O2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? O2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? C24 C23 C19 116.1(4) . . ? C24 C23 H23B 108.3 . . ? C19 C23 H23B 108.3 . . ? C24 C23 H23A 108.3 . . ? C19 C23 H23A 108.3 . . ? H23B C23 H23A 107.4 . . ? C29 C24 C25 118.2(5) . . ? C29 C24 C23 120.9(5) . . ? C25 C24 C23 120.8(4) . . ? C24 C25 O3 119.9(4) . . ? C24 C25 C26 121.7(4) . . ? O3 C25 C26 118.3(5) . . ? C27 C26 C25 117.3(5) . . ? C27 C26 C31 121.7(5) . . ? C25 C26 C31 121.0(5) . . ? O4 C27 C26 118.0(4) . . ? O4 C27 C28 118.9(4) . . ? C26 C27 C28 123.1(5) . . ? C27 C28 C29 116.5(4) . . ? C27 C28 C33 121.9(4) . . ? C29 C28 C33 121.6(4) . . ? C24 C29 C28 123.2(5) . . ? C24 C29 H29 118.4 . . ? C28 C29 H29 118.4 . . ? O3 C30 H30B 109.5 . . ? O3 C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O3 C30 H30A 109.5 . . ? H30B C30 H30A 109.5 . . ? H30C C30 H30A 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O4 C32 H32B 109.5 . . ? O4 C32 H32A 109.5 . . ? H32B C32 H32A 109.5 . . ? O4 C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? C3 C33 C28 115.8(4) 2 . ? C3 C33 H33A 108.3 2 . ? C28 C33 H33A 108.3 . . ? C3 C33 H33B 108.3 2 . ? C28 C33 H33B 108.3 . . ? H33A C33 H33B 107.4 . . ? C35 C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C35 C34 H34A 109.5 . . ? H34B C34 H34A 109.5 . . ? H34C C34 H34A 109.5 . . ? O5 C35 C36 122.4(9) . . ? O5 C35 C34 119.5(9) . . ? C36 C35 C34 118.2(9) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? H36C C36 H36B 109.5 . . ? C37A O6A C37A 18.8(11) . 2 ? C37A C37A O6A 121.7(11) 2 . ? C37A C37A O6A 39.5(7) 2 2 ? O6A C37A O6A 83.1(13) . 2 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 O1 C2 C7 81.2(6) . . . . ? C1 O1 C2 C3 -100.0(5) . . . . ? C7 C2 C3 C4 0.4(7) . . . . ? O1 C2 C3 C4 -178.4(4) . . . . ? C7 C2 C3 C33 -176.7(4) . . . 2 ? O1 C2 C3 C33 4.5(7) . . . 2 ? C2 C3 C4 C5 -0.5(7) . . . . ? C33 C3 C4 C5 176.7(5) 2 . . . ? C3 C4 C5 C6 0.5(8) . . . . ? C4 C5 C6 C7 -0.4(7) . . . . ? C4 C5 C6 C15 -179.3(5) . . . . ? O1 C2 C7 C6 178.5(4) . . . . ? C3 C2 C7 C6 -0.3(7) . . . . ? O1 C2 C7 C8 -2.3(7) . . . . ? C3 C2 C7 C8 178.9(4) . . . . ? C5 C6 C7 C2 0.3(7) . . . . ? C15 C6 C7 C2 179.4(4) . . . . ? C5 C6 C7 C8 -179.0(4) . . . . ? C15 C6 C7 C8 0.0(6) . . . . ? C2 C7 C8 C9 -123.5(5) . . . . ? C6 C7 C8 C9 55.8(5) . . . . ? C2 C7 C8 C17 124.4(5) . . . . ? C6 C7 C8 C17 -56.3(5) . . . . ? C7 C8 C9 C10 122.7(5) . . . . ? C17 C8 C9 C10 -125.7(5) . . . . ? C7 C8 C9 C14 -55.2(5) . . . . ? C17 C8 C9 C14 56.4(5) . . . . ? C14 C9 C10 C11 -0.4(7) . . . . ? C8 C9 C10 C11 -178.2(5) . . . . ? C9 C10 C11 C12 -1.7(8) . . . . ? C10 C11 C12 C13 1.9(9) . . . . ? C11 C12 C13 C14 0.0(8) . . . . ? C12 C13 C14 C9 -2.0(8) . . . . ? C12 C13 C14 C15 179.5(5) . . . . ? C10 C9 C14 C13 2.2(7) . . . . ? C8 C9 C14 C13 -179.7(5) . . . . ? C10 C9 C14 C15 -179.1(4) . . . . ? C8 C9 C14 C15 -1.0(6) . . . . ? C5 C6 C15 C14 123.0(5) . . . . ? C7 C6 C15 C14 -56.0(5) . . . . ? C5 C6 C15 C16 -125.2(5) . . . . ? C7 C6 C15 C16 55.7(5) . . . . ? C13 C14 C15 C6 -124.8(5) . . . . ? C9 C14 C15 C6 56.6(5) . . . . ? C13 C14 C15 C16 123.3(5) . . . . ? C9 C14 C15 C16 -55.3(5) . . . . ? C6 C15 C16 C21 125.5(5) . . . . ? C14 C15 C16 C21 -123.2(5) . . . . ? C6 C15 C16 C17 -54.6(5) . . . . ? C14 C15 C16 C17 56.6(5) . . . . ? C21 C16 C17 C18 -1.9(7) . . . . ? C15 C16 C17 C18 178.2(4) . . . . ? C21 C16 C17 C8 178.3(4) . . . . ? C15 C16 C17 C8 -1.6(5) . . . . ? C7 C8 C17 C18 -122.7(5) . . . . ? C9 C8 C17 C18 125.6(5) . . . . ? C7 C8 C17 C16 57.0(5) . . . . ? C9 C8 C17 C16 -54.7(5) . . . . ? C16 C17 C18 O2 178.1(4) . . . . ? C8 C17 C18 O2 -2.2(7) . . . . ? C16 C17 C18 C19 1.1(7) . . . . ? C8 C17 C18 C19 -179.2(4) . . . . ? C22 O2 C18 C17 78.6(5) . . . . ? C22 O2 C18 C19 -104.4(5) . . . . ? C17 C18 C19 C20 0.1(7) . . . . ? O2 C18 C19 C20 -176.9(4) . . . . ? C17 C18 C19 C23 -177.5(4) . . . . ? O2 C18 C19 C23 5.5(6) . . . . ? C18 C19 C20 C21 -0.5(7) . . . . ? C23 C19 C20 C21 177.0(5) . . . . ? C17 C16 C21 C20 1.6(7) . . . . ? C15 C16 C21 C20 -178.6(4) . . . . ? C19 C20 C21 C16 -0.4(7) . . . . ? C20 C19 C23 C24 0.4(7) . . . . ? C18 C19 C23 C24 177.8(4) . . . . ? C19 C23 C24 C29 -89.4(6) . . . . ? C19 C23 C24 C25 91.6(6) . . . . ? C29 C24 C25 O3 -176.1(4) . . . . ? C23 C24 C25 O3 3.0(7) . . . . ? C29 C24 C25 C26 -0.4(7) . . . . ? C23 C24 C25 C26 178.7(4) . . . . ? C30 O3 C25 C24 -93.1(6) . . . . ? C30 O3 C25 C26 91.0(6) . . . . ? C24 C25 C26 C27 -0.5(7) . . . . ? O3 C25 C26 C27 175.2(4) . . . . ? C24 C25 C26 C31 178.8(5) . . . . ? O3 C25 C26 C31 -5.5(7) . . . . ? C32 O4 C27 C26 91.5(6) . . . . ? C32 O4 C27 C28 -90.6(6) . . . . ? C25 C26 C27 O4 179.2(4) . . . . ? C31 C26 C27 O4 -0.1(7) . . . . ? C25 C26 C27 C28 1.3(7) . . . . ? C31 C26 C27 C28 -177.9(5) . . . . ? O4 C27 C28 C29 -179.0(4) . . . . ? C26 C27 C28 C29 -1.2(8) . . . . ? O4 C27 C28 C33 1.3(8) . . . . ? C26 C27 C28 C33 179.1(5) . . . . ? C25 C24 C29 C28 0.5(7) . . . . ? C23 C24 C29 C28 -178.6(5) . . . . ? C27 C28 C29 C24 0.3(8) . . . . ? C33 C28 C29 C24 179.9(5) . . . . ? C27 C28 C33 C3 -139.6(5) . . . 2 ? C29 C28 C33 C3 40.7(7) . . . 2 ? C37A O6A C37A O6A 9(5) 2 . . 2 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.696 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.155 _database_code_depnum_ccdc_archive 'CCDC 931895' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sa2444 #TrackingRef 'web_deposit_cif_file_1_Taoxie_1364731106.sa2444.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H60 O8, 2(C H Cl3)' _chemical_formula_sum 'C68 H62 Cl6 O8' _chemical_formula_weight 1219.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.466(2) _cell_length_b 11.708(2) _cell_length_c 13.256(3) _cell_angle_alpha 69.828(9) _cell_angle_beta 73.892(9) _cell_angle_gamma 72.609(9) _cell_volume 1563.5(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5256 _cell_measurement_theta_min 1.90 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 0.329 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6566 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16948 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5487 _reflns_number_gt 4660 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'Olex2 ver 1.1' _computing_molecular_graphics 'Olex2 ver 1.1' _computing_publication_material 'SHELX97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1417P)^2^+2.1755P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5487 _refine_ls_number_parameters 394 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0849 _refine_ls_wR_factor_ref 0.2403 _refine_ls_wR_factor_gt 0.2311 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.77242(13) 0.36734(14) 0.35494(10) 0.0758(4) Uani 1 1 d . . . Cl2 Cl 0.63245(12) 0.59448(12) 0.22663(10) 0.0694(4) Uani 1 1 d . . . Cl3 Cl 0.77205(14) 0.39634(13) 0.12926(10) 0.0761(4) Uani 1 1 d . . . O1 O 1.9753(2) 0.2898(2) -0.4501(2) 0.0442(6) Uani 1 1 d . . . O2 O 1.9353(2) 0.3263(2) -0.0909(2) 0.0465(6) Uani 1 1 d . . . O3 O 1.7042(3) 0.0237(3) 0.2288(3) 0.0715(11) Uani 1 1 d D . . O4 O 1.3268(3) -0.0648(2) 0.4036(2) 0.0569(8) Uani 1 1 d D . . C1 C 1.9339(3) 0.2580(3) -0.1573(3) 0.0348(7) Uani 1 1 d . . . C2 C 1.9678(3) 0.3054(3) -0.2713(3) 0.0376(7) Uani 1 1 d . . . C3 C 1.9556(3) 0.2396(3) -0.3366(3) 0.0365(7) Uani 1 1 d . . . C4 C 1.9152(3) 0.1271(3) -0.2906(3) 0.0395(8) Uani 1 1 d . . . C5 C 1.8811(3) 0.0858(3) -0.1773(3) 0.0382(8) Uani 1 1 d . . . H5 H 1.8520 0.0108 -0.1453 0.046 Uiso 1 1 calc R . . C6 C 1.8879(3) 0.1497(3) -0.1089(3) 0.0352(7) Uani 1 1 d . . . C7 C 2.0557(5) 0.3077(6) -0.0678(4) 0.0711(13) Uani 1 1 d . . . H7A H 2.0557 0.3744 -0.0390 0.107 Uiso 1 1 calc R . . H7B H 2.1188 0.3092 -0.1352 0.107 Uiso 1 1 calc R . . H7C H 2.0750 0.2268 -0.0132 0.107 Uiso 1 1 calc R . . C8 C 2.0099(4) 0.4254(4) -0.3223(3) 0.0516(9) Uani 1 1 d . . . H8A H 1.9715 0.4798 -0.2743 0.077 Uiso 1 1 calc R . . H8B H 1.9849 0.4669 -0.3936 0.077 Uiso 1 1 calc R . . H8C H 2.1008 0.4083 -0.3324 0.077 Uiso 1 1 calc R . . C9 C 2.1000(4) 0.2620(4) -0.5030(3) 0.0545(10) Uani 1 1 d . . . H9A H 2.1056 0.2951 -0.5825 0.082 Uiso 1 1 calc R . . H9B H 2.1319 0.1713 -0.4835 0.082 Uiso 1 1 calc R . . H9C H 2.1497 0.3002 -0.4800 0.082 Uiso 1 1 calc R . . C10 C 1.8405(3) 0.1064(3) 0.0129(3) 0.0390(8) Uani 1 1 d . A . H10A H 1.8954 0.1206 0.0511 0.047 Uiso 1 1 calc R . . H10B H 1.8461 0.0154 0.0349 0.047 Uiso 1 1 calc R . . C11 C 1.7063(3) 0.1717(3) 0.0508(3) 0.0323(7) Uani 1 1 d . . . C12 C 1.6430(3) 0.2767(3) -0.0195(2) 0.0321(7) Uani 1 1 d . A . H12 H 1.6824 0.3052 -0.0938 0.038 Uiso 1 1 calc R . . C13 C 1.5239(3) 0.3402(3) 0.0171(2) 0.0316(7) Uani 1 1 d . . . H13 H 1.4828 0.4118 -0.0317 0.038 Uiso 1 1 calc R A . C14 C 1.4653(3) 0.2986(3) 0.1248(2) 0.0298(6) Uani 1 1 d . A . C15 C 1.5253(3) 0.1902(3) 0.1951(2) 0.0314(7) Uani 1 1 d . . . C16 C 1.6441(3) 0.1288(3) 0.1581(3) 0.0354(7) Uani 1 1 d . A . C17 C 1.7600(8) 0.0287(9) 0.2912(7) 0.061(3) Uani 0.505(11) 1 d PDU A 1 H17A H 1.7951 -0.0561 0.3330 0.091 Uiso 0.505(11) 1 calc PR A 1 H17B H 1.7028 0.0746 0.3418 0.091 Uiso 0.505(11) 1 calc PR A 1 H17C H 1.8274 0.0718 0.2498 0.091 Uiso 0.505(11) 1 calc PR A 1 C17' C 1.7023(9) -0.0837(7) 0.2508(7) 0.059(3) Uani 0.495(11) 1 d PDU A 2 H17D H 1.7563 -0.1343 0.3037 0.088 Uiso 0.495(11) 1 calc PR A 2 H17E H 1.7323 -0.1108 0.1841 0.088 Uiso 0.495(11) 1 calc PR A 2 H17F H 1.6169 -0.0943 0.2827 0.088 Uiso 0.495(11) 1 calc PR A 2 C18 C 1.4441(3) 0.1527(3) 0.3094(3) 0.0357(7) Uani 1 1 d . A . H18 H 1.4851 0.0740 0.3592 0.043 Uiso 1 1 calc R . . C19 C 1.4128(3) 0.2660(3) 0.3522(3) 0.0350(7) Uani 1 1 d . . . C20 C 1.3548(3) 0.3762(3) 0.2822(2) 0.0312(7) Uani 1 1 d . A . C21 C 1.3369(3) 0.3578(3) 0.1798(2) 0.0304(7) Uani 1 1 d . . . H21 H 1.2956 0.4365 0.1302 0.036 Uiso 1 1 calc R A . C22 C 1.3176(3) 0.4864(3) 0.3104(3) 0.0375(7) Uani 1 1 d . . . H22 H 1.2783 0.5610 0.2632 0.045 Uiso 1 1 calc R A . C23 C 1.3381(4) 0.4872(4) 0.4092(3) 0.0519(10) Uani 1 1 d . A . H23 H 1.3126 0.5629 0.4290 0.062 Uiso 1 1 calc R . . C24 C 1.3952(4) 0.3787(4) 0.4787(3) 0.0554(10) Uani 1 1 d . . . H24 H 1.4084 0.3802 0.5458 0.066 Uiso 1 1 calc R A . C25 C 1.4333(3) 0.2673(4) 0.4497(3) 0.0470(9) Uani 1 1 d . A . H25 H 1.4730 0.1928 0.4968 0.056 Uiso 1 1 calc R . . C26 C 1.2630(3) 0.2560(3) 0.2222(3) 0.0328(7) Uani 1 1 d . A . C27 C 1.3220(3) 0.1454(3) 0.2907(3) 0.0343(7) Uani 1 1 d . . . C28 C 1.2673(3) 0.0436(3) 0.3354(3) 0.0421(8) Uani 1 1 d . A . C29 C 1.1512(3) 0.0511(4) 0.3162(3) 0.0446(9) Uani 1 1 d . . . C30 C 1.0928(3) 0.1632(4) 0.2507(3) 0.0468(9) Uani 1 1 d . A . H30 H 1.0129 0.1701 0.2382 0.056 Uiso 1 1 calc R . . C31 C 1.1479(3) 0.2660(3) 0.2025(3) 0.0392(8) Uani 1 1 d . . . H31 H 1.1068 0.3412 0.1572 0.047 Uiso 1 1 calc R A . C32 C 1.0886(4) -0.0588(4) 0.3681(3) 0.0556(11) Uani 1 1 d . . . H32A H 1.0020 -0.0282 0.4036 0.067 Uiso 1 1 calc R . . H32B H 1.1326 -0.1194 0.4264 0.067 Uiso 1 1 calc R . . C33 C 1.2937(8) -0.0598(8) 0.5289(6) 0.040(2) Uani 0.424(11) 1 d PDU B 1 H33A H 1.3214 0.0100 0.5324 0.060 Uiso 0.424(11) 1 calc PR B 1 H33B H 1.3362 -0.1382 0.5746 0.060 Uiso 0.424(11) 1 calc PR B 1 H33C H 1.2035 -0.0481 0.5557 0.060 Uiso 0.424(11) 1 calc PR B 1 C33' C 1.3901(8) -0.1557(7) 0.3307(7) 0.063(2) Uani 0.576(11) 1 d PDU B 2 H33D H 1.4340 -0.2349 0.3743 0.094 Uiso 0.576(11) 1 calc PR B 2 H33E H 1.4495 -0.1180 0.2682 0.094 Uiso 0.576(11) 1 calc PR B 2 H33F H 1.3262 -0.1711 0.3041 0.094 Uiso 0.576(11) 1 calc PR B 2 C34 C 0.6841(4) 0.4314(5) 0.2513(4) 0.0601(11) Uani 1 1 d . . . H34 H 0.6096 0.3940 0.2757 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0800(8) 0.0910(9) 0.0563(7) -0.0250(6) -0.0148(6) -0.0128(7) Cl2 0.0664(7) 0.0799(8) 0.0673(7) -0.0318(6) -0.0086(5) -0.0157(6) Cl3 0.0990(10) 0.0843(9) 0.0630(7) -0.0403(6) -0.0130(6) -0.0264(7) O1 0.0445(14) 0.0482(14) 0.0354(13) -0.0079(10) -0.0010(10) -0.0154(11) O2 0.0511(15) 0.0549(15) 0.0406(14) -0.0174(11) -0.0041(11) -0.0223(12) O3 0.0508(17) 0.055(2) 0.0491(17) 0.0195(14) 0.0103(14) 0.0149(14) O4 0.0528(16) 0.0339(13) 0.0639(18) -0.0037(12) 0.0084(13) -0.0112(11) C1 0.0283(15) 0.0412(17) 0.0350(17) -0.0135(14) -0.0008(12) -0.0096(13) C2 0.0333(17) 0.0418(18) 0.0366(18) -0.0122(14) 0.0032(13) -0.0150(14) C3 0.0327(16) 0.0439(18) 0.0298(16) -0.0120(14) 0.0048(13) -0.0125(14) C4 0.0340(17) 0.0443(19) 0.0408(18) -0.0181(15) 0.0059(14) -0.0150(14) C5 0.0326(16) 0.0390(17) 0.0394(18) -0.0127(14) 0.0081(13) -0.0152(13) C6 0.0238(15) 0.0377(17) 0.0373(17) -0.0100(14) 0.0013(12) -0.0047(12) C7 0.060(3) 0.102(4) 0.072(3) -0.031(3) -0.019(2) -0.034(3) C8 0.060(2) 0.051(2) 0.047(2) -0.0153(17) 0.0025(18) -0.0270(19) C9 0.053(2) 0.058(2) 0.043(2) -0.0117(18) 0.0092(17) -0.0187(19) C10 0.0341(17) 0.0405(18) 0.0352(17) -0.0089(14) -0.0006(13) -0.0061(14) C11 0.0306(16) 0.0323(16) 0.0337(16) -0.0099(13) -0.0039(13) -0.0081(12) C12 0.0353(16) 0.0357(16) 0.0249(14) -0.0097(12) -0.0005(12) -0.0112(13) C13 0.0366(17) 0.0300(15) 0.0281(15) -0.0065(12) -0.0087(12) -0.0072(12) C14 0.0310(15) 0.0280(15) 0.0313(16) -0.0101(12) -0.0044(12) -0.0077(12) C15 0.0322(16) 0.0318(15) 0.0258(15) -0.0061(12) -0.0005(12) -0.0082(12) C16 0.0337(17) 0.0280(16) 0.0376(18) -0.0027(13) -0.0054(13) -0.0060(13) C17 0.043(4) 0.076(6) 0.047(5) 0.008(4) -0.026(4) -0.005(4) C17' 0.068(6) 0.043(5) 0.051(5) 0.001(4) -0.016(4) -0.006(4) C18 0.0313(16) 0.0349(16) 0.0315(16) -0.0025(13) -0.0018(13) -0.0061(13) C19 0.0273(15) 0.0443(18) 0.0283(15) -0.0063(13) 0.0015(12) -0.0118(13) C20 0.0290(15) 0.0361(16) 0.0282(15) -0.0081(12) -0.0009(12) -0.0122(12) C21 0.0313(16) 0.0302(15) 0.0281(15) -0.0071(12) -0.0054(12) -0.0066(12) C22 0.0360(17) 0.0408(18) 0.0371(17) -0.0162(14) 0.0007(13) -0.0116(14) C23 0.056(2) 0.065(2) 0.047(2) -0.0310(19) -0.0013(17) -0.0203(19) C24 0.055(2) 0.083(3) 0.037(2) -0.024(2) -0.0073(17) -0.022(2) C25 0.0399(19) 0.065(2) 0.0329(18) -0.0076(16) -0.0074(14) -0.0139(17) C26 0.0345(16) 0.0366(16) 0.0298(15) -0.0164(13) -0.0015(12) -0.0079(13) C27 0.0290(15) 0.0336(16) 0.0352(17) -0.0113(13) 0.0043(12) -0.0075(12) C28 0.0377(18) 0.0348(17) 0.046(2) -0.0140(15) 0.0110(15) -0.0116(14) C29 0.044(2) 0.049(2) 0.044(2) -0.0256(16) 0.0118(15) -0.0199(16) C30 0.0377(18) 0.068(2) 0.048(2) -0.0344(19) 0.0022(15) -0.0196(17) C31 0.0343(17) 0.0465(19) 0.0418(18) -0.0231(15) -0.0028(14) -0.0084(14) C32 0.062(2) 0.068(3) 0.047(2) -0.027(2) 0.0161(18) -0.041(2) C33 0.041(4) 0.049(5) 0.027(4) -0.011(3) -0.005(3) -0.008(3) C33' 0.071(5) 0.044(4) 0.085(6) -0.033(4) -0.034(4) 0.003(3) C34 0.058(3) 0.076(3) 0.060(3) -0.024(2) -0.004(2) -0.035(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C34 1.756(5) . ? Cl2 C34 1.761(5) . ? Cl3 C34 1.763(5) . ? O1 C3 1.393(4) . ? O1 C9 1.401(5) . ? O2 C1 1.384(4) . ? O2 C7 1.435(5) . ? O3 C17' 1.194(8) . ? O3 C17 1.203(8) . ? O3 C16 1.387(4) . ? O4 C28 1.388(5) . ? O4 C33' 1.566(7) . ? O4 C33 1.615(8) . ? C1 C6 1.396(5) . ? C1 C2 1.403(5) . ? C2 C3 1.397(5) . ? C2 C8 1.495(5) . ? C3 C4 1.405(5) . ? C4 C5 1.388(5) . ? C4 C32 1.520(5) 2_855 ? C5 C6 1.390(5) . ? C5 H5 0.9500 . ? C6 C10 1.508(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.528(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.394(5) . ? C11 C12 1.400(4) . ? C12 C13 1.388(5) . ? C12 H12 0.9500 . ? C13 C14 1.382(4) . ? C13 H13 0.9500 . ? C14 C15 1.404(4) . ? C14 C21 1.524(4) . ? C15 C16 1.378(5) . ? C15 C18 1.536(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17' H17D 0.9800 . ? C17' H17E 0.9800 . ? C17' H17F 0.9800 . ? C18 C27 1.519(5) . ? C18 C19 1.527(5) . ? C18 H18 1.0000 . ? C19 C25 1.382(5) . ? C19 C20 1.404(5) . ? C20 C22 1.379(5) . ? C20 C21 1.521(4) . ? C21 C26 1.528(4) . ? C21 H21 1.0000 . ? C22 C23 1.396(5) . ? C22 H22 0.9500 . ? C23 C24 1.385(6) . ? C23 H23 0.9500 . ? C24 C25 1.397(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.379(5) . ? C26 C27 1.402(5) . ? C27 C28 1.385(5) . ? C28 C29 1.396(6) . ? C29 C30 1.392(6) . ? C29 C32 1.519(5) . ? C30 C31 1.398(5) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C4 1.520(5) 2_855 ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C33' H33D 0.9800 . ? C33' H33E 0.9800 . ? C33' H33F 0.9800 . ? C34 H34 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 O1 C9 114.3(3) . . ? C1 O2 C7 113.9(3) . . ? C17' O3 C17 105.9(7) . . ? C17' O3 C16 130.5(6) . . ? C17 O3 C16 123.2(6) . . ? C28 O4 C33' 105.2(4) . . ? C28 O4 C33 111.9(4) . . ? C33' O4 C33 142.3(5) . . ? O2 C1 C6 118.6(3) . . ? O2 C1 C2 119.1(3) . . ? C6 C1 C2 122.1(3) . . ? C3 C2 C1 117.8(3) . . ? C3 C2 C8 120.7(3) . . ? C1 C2 C8 121.5(3) . . ? O1 C3 C2 119.9(3) . . ? O1 C3 C4 118.3(3) . . ? C2 C3 C4 121.7(3) . . ? C5 C4 C3 117.9(3) . . ? C5 C4 C32 124.2(3) . 2_855 ? C3 C4 C32 117.9(3) . 2_855 ? C4 C5 C6 122.6(3) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 117.8(3) . . ? C5 C6 C10 120.6(3) . . ? C1 C6 C10 121.5(3) . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 H9A 109.5 . . ? O1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C11 114.1(3) . . ? C6 C10 H10A 108.7 . . ? C11 C10 H10A 108.7 . . ? C6 C10 H10B 108.7 . . ? C11 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C16 C11 C12 118.0(3) . . ? C16 C11 C10 120.4(3) . . ? C12 C11 C10 121.6(3) . . ? C13 C12 C11 121.4(3) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C12 119.7(3) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 119.6(3) . . ? C13 C14 C21 127.0(3) . . ? C15 C14 C21 113.4(3) . . ? C16 C15 C14 120.1(3) . . ? C16 C15 C18 127.1(3) . . ? C14 C15 C18 112.8(3) . . ? C15 C16 O3 119.8(3) . . ? C15 C16 C11 121.1(3) . . ? O3 C16 C11 119.1(3) . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O3 C17' H17D 109.5 . . ? O3 C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? O3 C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? C27 C18 C19 105.6(3) . . ? C27 C18 C15 105.9(3) . . ? C19 C18 C15 104.8(3) . . ? C27 C18 H18 113.2 . . ? C19 C18 H18 113.2 . . ? C15 C18 H18 113.2 . . ? C25 C19 C20 120.2(3) . . ? C25 C19 C18 126.7(3) . . ? C20 C19 C18 113.0(3) . . ? C22 C20 C19 120.2(3) . . ? C22 C20 C21 126.3(3) . . ? C19 C20 C21 113.5(3) . . ? C20 C21 C14 106.3(2) . . ? C20 C21 C26 105.0(2) . . ? C14 C21 C26 105.3(2) . . ? C20 C21 H21 113.2 . . ? C14 C21 H21 113.2 . . ? C26 C21 H21 113.2 . . ? C20 C22 C23 119.4(3) . . ? C20 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C24 C23 C22 120.7(4) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 119.9(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C19 C25 C24 119.6(4) . . ? C19 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C31 C26 C27 120.3(3) . . ? C31 C26 C21 126.7(3) . . ? C27 C26 C21 112.9(3) . . ? C28 C27 C26 120.1(3) . . ? C28 C27 C18 126.3(3) . . ? C26 C27 C18 113.6(3) . . ? C27 C28 O4 119.2(3) . . ? C27 C28 C29 120.7(3) . . ? O4 C28 C29 120.1(3) . . ? C30 C29 C28 118.1(3) . . ? C30 C29 C32 121.0(4) . . ? C28 C29 C32 121.0(4) . . ? C29 C30 C31 122.1(3) . . ? C29 C30 H30 118.9 . . ? C31 C30 H30 118.9 . . ? C26 C31 C30 118.7(3) . . ? C26 C31 H31 120.7 . . ? C30 C31 H31 120.7 . . ? C29 C32 C4 115.8(3) . 2_855 ? C29 C32 H32A 108.3 . . ? C4 C32 H32A 108.3 2_855 . ? C29 C32 H32B 108.3 . . ? C4 C32 H32B 108.3 2_855 . ? H32A C32 H32B 107.4 . . ? O4 C33 H33A 109.5 . . ? O4 C33 H33B 109.5 . . ? O4 C33 H33C 109.5 . . ? O4 C33' H33D 109.5 . . ? O4 C33' H33E 109.5 . . ? H33D C33' H33E 109.5 . . ? O4 C33' H33F 109.5 . . ? H33D C33' H33F 109.5 . . ? H33E C33' H33F 109.5 . . ? Cl1 C34 Cl2 110.8(2) . . ? Cl1 C34 Cl3 110.6(3) . . ? Cl2 C34 Cl3 109.8(3) . . ? Cl1 C34 H34 108.5 . . ? Cl2 C34 H34 108.5 . . ? Cl3 C34 H34 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 O2 C1 C6 102.1(4) . . . . ? C7 O2 C1 C2 -83.6(4) . . . . ? O2 C1 C2 C3 -174.8(3) . . . . ? C6 C1 C2 C3 -0.7(5) . . . . ? O2 C1 C2 C8 2.3(5) . . . . ? C6 C1 C2 C8 176.4(3) . . . . ? C9 O1 C3 C2 86.6(4) . . . . ? C9 O1 C3 C4 -97.8(4) . . . . ? C1 C2 C3 O1 173.2(3) . . . . ? C8 C2 C3 O1 -3.9(5) . . . . ? C1 C2 C3 C4 -2.3(5) . . . . ? C8 C2 C3 C4 -179.4(3) . . . . ? O1 C3 C4 C5 -172.3(3) . . . . ? C2 C3 C4 C5 3.3(5) . . . . ? O1 C3 C4 C32 7.6(5) . . . 2_855 ? C2 C3 C4 C32 -176.8(3) . . . 2_855 ? C3 C4 C5 C6 -1.3(5) . . . . ? C32 C4 C5 C6 178.8(3) 2_855 . . . ? C4 C5 C6 C1 -1.6(5) . . . . ? C4 C5 C6 C10 175.2(3) . . . . ? O2 C1 C6 C5 176.7(3) . . . . ? C2 C1 C6 C5 2.6(5) . . . . ? O2 C1 C6 C10 -0.1(5) . . . . ? C2 C1 C6 C10 -174.2(3) . . . . ? C5 C6 C10 C11 -94.6(4) . . . . ? C1 C6 C10 C11 82.1(4) . . . . ? C6 C10 C11 C16 170.5(3) . . . . ? C6 C10 C11 C12 -10.6(5) . . . . ? C16 C11 C12 C13 2.9(5) . . . . ? C10 C11 C12 C13 -176.1(3) . . . . ? C11 C12 C13 C14 -0.7(5) . . . . ? C12 C13 C14 C15 -2.2(5) . . . . ? C12 C13 C14 C21 178.4(3) . . . . ? C13 C14 C15 C16 2.9(5) . . . . ? C21 C14 C15 C16 -177.6(3) . . . . ? C13 C14 C15 C18 -176.4(3) . . . . ? C21 C14 C15 C18 3.1(4) . . . . ? C14 C15 C16 O3 178.2(3) . . . . ? C18 C15 C16 O3 -2.7(6) . . . . ? C14 C15 C16 C11 -0.6(5) . . . . ? C18 C15 C16 C11 178.5(3) . . . . ? C17' O3 C16 C15 87.2(8) . . . . ? C17 O3 C16 C15 -83.7(7) . . . . ? C17' O3 C16 C11 -93.9(7) . . . . ? C17 O3 C16 C11 95.1(6) . . . . ? C12 C11 C16 C15 -2.2(5) . . . . ? C10 C11 C16 C15 176.8(3) . . . . ? C12 C11 C16 O3 179.0(3) . . . . ? C10 C11 C16 O3 -2.0(5) . . . . ? C16 C15 C18 C27 -125.7(3) . . . . ? C14 C15 C18 C27 53.5(3) . . . . ? C16 C15 C18 C19 122.9(4) . . . . ? C14 C15 C18 C19 -58.0(3) . . . . ? C27 C18 C19 C25 123.0(4) . . . . ? C15 C18 C19 C25 -125.3(3) . . . . ? C27 C18 C19 C20 -55.4(3) . . . . ? C15 C18 C19 C20 56.3(3) . . . . ? C25 C19 C20 C22 -0.2(5) . . . . ? C18 C19 C20 C22 178.3(3) . . . . ? C25 C19 C20 C21 -178.8(3) . . . . ? C18 C19 C20 C21 -0.3(4) . . . . ? C22 C20 C21 C14 126.4(3) . . . . ? C19 C20 C21 C14 -55.1(3) . . . . ? C22 C20 C21 C26 -122.3(3) . . . . ? C19 C20 C21 C26 56.1(3) . . . . ? C13 C14 C21 C20 -127.2(3) . . . . ? C15 C14 C21 C20 53.3(3) . . . . ? C13 C14 C21 C26 121.8(3) . . . . ? C15 C14 C21 C26 -57.7(3) . . . . ? C19 C20 C22 C23 0.0(5) . . . . ? C21 C20 C22 C23 178.4(3) . . . . ? C20 C22 C23 C24 0.0(6) . . . . ? C22 C23 C24 C25 0.3(6) . . . . ? C20 C19 C25 C24 0.4(5) . . . . ? C18 C19 C25 C24 -177.8(3) . . . . ? C23 C24 C25 C19 -0.5(6) . . . . ? C20 C21 C26 C31 120.7(3) . . . . ? C14 C21 C26 C31 -127.3(3) . . . . ? C20 C21 C26 C27 -56.8(3) . . . . ? C14 C21 C26 C27 55.2(3) . . . . ? C31 C26 C27 C28 2.7(5) . . . . ? C21 C26 C27 C28 -179.6(3) . . . . ? C31 C26 C27 C18 -176.3(3) . . . . ? C21 C26 C27 C18 1.4(4) . . . . ? C19 C18 C27 C28 -124.2(3) . . . . ? C15 C18 C27 C28 124.9(3) . . . . ? C19 C18 C27 C26 54.7(3) . . . . ? C15 C18 C27 C26 -56.1(3) . . . . ? C26 C27 C28 O4 -179.6(3) . . . . ? C18 C27 C28 O4 -0.7(5) . . . . ? C26 C27 C28 C29 -2.3(5) . . . . ? C18 C27 C28 C29 176.6(3) . . . . ? C33' O4 C28 C27 -101.7(5) . . . . ? C33 O4 C28 C27 85.2(5) . . . . ? C33' O4 C28 C29 80.9(5) . . . . ? C33 O4 C28 C29 -92.1(5) . . . . ? C27 C28 C29 C30 0.3(5) . . . . ? O4 C28 C29 C30 177.6(3) . . . . ? C27 C28 C29 C32 -178.0(3) . . . . ? O4 C28 C29 C32 -0.7(5) . . . . ? C28 C29 C30 C31 1.3(5) . . . . ? C32 C29 C30 C31 179.6(3) . . . . ? C27 C26 C31 C30 -1.1(5) . . . . ? C21 C26 C31 C30 -178.4(3) . . . . ? C29 C30 C31 C26 -0.9(5) . . . . ? C30 C29 C32 C4 73.5(5) . . . 2_855 ? C28 C29 C32 C4 -108.3(4) . . . 2_855 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.049 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.093 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 1.000 101 41 ' ' _database_code_depnum_ccdc_archive 'CCDC 931896' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a2 #TrackingRef 'web_deposit_cif_file_2_Taoxie_1364731106.a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H60 O10' _chemical_formula_sum 'C66 H60 O10' _chemical_formula_weight 1013.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.429(2) _cell_length_b 11.955(2) _cell_length_c 12.714(3) _cell_angle_alpha 72.18(3) _cell_angle_beta 70.44(3) _cell_angle_gamma 70.84(3) _cell_volume 1508.3(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5176 _cell_measurement_theta_min 1.7426 _cell_measurement_theta_max 27.4825 _exptl_crystal_description plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.115 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7584 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007HF + CCD (Saturn724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19654 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6896 _reflns_number_gt 5476 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1531P)^2^+1.7889P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6896 _refine_ls_number_parameters 348 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1111 _refine_ls_R_factor_gt 0.0974 _refine_ls_wR_factor_ref 0.2907 _refine_ls_wR_factor_gt 0.2766 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.7083(3) 0.6068(2) 0.5443(2) 0.0442(6) Uani 1 1 d . . . O2 O 0.6277(2) 0.4936(2) 0.7707(2) 0.0359(5) Uani 1 1 d . . . O3 O 0.7783(2) 0.45364(19) 0.92152(18) 0.0306(5) Uani 1 1 d . . . O4 O 1.00401(19) 0.84711(18) 0.23832(17) 0.0261(4) Uani 1 1 d . . . O5 O 1.0453(2) 1.2309(2) 0.08077(18) 0.0302(5) Uani 1 1 d . . . C1 C 0.6888(4) 0.5029(4) 0.5273(4) 0.0515(10) Uani 1 1 d . . . H1C H 0.7720 0.4466 0.5036 0.077 Uiso 1 1 calc R . . H1A H 0.6431 0.5278 0.4677 0.077 Uiso 1 1 calc R . . H1B H 0.6378 0.4626 0.5989 0.077 Uiso 1 1 calc R . . C2 C 0.6380(4) 0.3664(4) 0.8210(4) 0.0484(9) Uani 1 1 d . . . H2C H 0.6451 0.3488 0.8994 0.073 Uiso 1 1 calc R . . H2B H 0.7145 0.3184 0.7757 0.073 Uiso 1 1 calc R . . H2A H 0.5616 0.3455 0.8220 0.073 Uiso 1 1 calc R . . C3 C 0.6709(4) 0.5234(4) 0.9925(3) 0.0415(8) Uani 1 1 d . . . H3A H 0.5984 0.5538 0.9579 0.062 Uiso 1 1 calc R . . H3C H 0.6946 0.5921 0.9993 0.062 Uiso 1 1 calc R . . H3B H 0.6465 0.4720 1.0686 0.062 Uiso 1 1 calc R . . C4 C 0.7805(3) 0.5859(3) 0.6187(3) 0.0318(7) Uani 1 1 d . . . C5 C 0.7416(3) 0.5275(3) 0.7336(3) 0.0319(7) Uani 1 1 d . . . C6 C 0.8125(3) 0.5154(2) 0.8088(2) 0.0264(6) Uani 1 1 d . . . C7 C 0.9208(3) 0.5599(2) 0.7721(2) 0.0261(6) Uani 1 1 d . . . C8 C 0.9939(3) 0.5440(3) 0.8580(2) 0.0287(6) Uani 1 1 d . . . H8B H 0.9313 0.5694 0.9274 0.034 Uiso 1 1 calc R . . H8A H 1.0347 0.4565 0.8807 0.034 Uiso 1 1 calc R . . C9 C 0.9568(3) 0.6175(3) 0.6568(2) 0.0266(6) Uani 1 1 d . . . H9 H 1.0302 0.6493 0.6306 0.032 Uiso 1 1 calc R . . C10 C 0.8897(3) 0.6301(3) 0.5797(2) 0.0270(6) Uani 1 1 d . . . C11 C 0.9335(3) 0.6923(3) 0.4556(2) 0.0292(6) Uani 1 1 d . . . H11A H 0.9326 0.6424 0.4066 0.035 Uiso 1 1 calc R . . H11B H 1.0232 0.6960 0.4397 0.035 Uiso 1 1 calc R . . C12 C 0.8520(3) 0.8203(3) 0.4226(2) 0.0245(6) Uani 1 1 d . . . C13 C 0.7402(3) 0.8718(3) 0.4974(2) 0.0295(6) Uani 1 1 d . . . H13 H 0.7156 0.8266 0.5734 0.035 Uiso 1 1 calc R . . C14 C 0.6636(3) 0.9866(3) 0.4650(3) 0.0288(6) Uani 1 1 d . . . H14 H 0.5876 1.0186 0.5180 0.035 Uiso 1 1 calc R . . C15 C 0.6985(3) 1.0536(3) 0.3555(2) 0.0245(6) Uani 1 1 d . . . C16 C 0.8141(3) 1.0084(2) 0.2802(2) 0.0221(5) Uani 1 1 d . . . C17 C 0.8896(3) 0.8920(2) 0.3132(2) 0.0220(5) Uani 1 1 d . . . C18 C 0.9875(3) 0.7900(3) 0.1617(3) 0.0346(7) Uani 1 1 d . . . H18C H 1.0710 0.7614 0.1102 0.052 Uiso 1 1 calc R . . H18B H 0.9297 0.8487 0.1167 0.052 Uiso 1 1 calc R . . H18A H 0.9508 0.7209 0.2060 0.052 Uiso 1 1 calc R . . C19 C 0.6238(3) 1.1771(3) 0.3021(3) 0.0287(6) Uani 1 1 d . . . H19 H 0.5400 1.2085 0.3552 0.034 Uiso 1 1 calc R . . C20 C 0.6088(3) 1.1597(3) 0.1938(2) 0.0250(6) Uani 1 1 d . . . C21 C 0.4949(3) 1.1774(3) 0.1686(3) 0.0336(7) Uani 1 1 d . . . H21 H 0.4153 1.2087 0.2181 0.040 Uiso 1 1 calc R . . C22 C 0.4986(3) 1.1487(3) 0.0690(3) 0.0374(7) Uani 1 1 d . . . H22 H 0.4206 1.1587 0.0517 0.045 Uiso 1 1 calc R . . C23 C 0.6150(3) 1.1055(3) -0.0055(3) 0.0358(7) Uani 1 1 d . . . H23 H 0.6158 1.0873 -0.0734 0.043 Uiso 1 1 calc R . . C24 C 0.7294(3) 1.0890(3) 0.0188(3) 0.0294(6) Uani 1 1 d . . . H24 H 0.8089 1.0599 -0.0321 0.035 Uiso 1 1 calc R . . C25 C 0.7266(3) 1.1155(2) 0.1189(2) 0.0248(6) Uani 1 1 d . . . C26 C 0.8420(3) 1.0949(2) 0.1638(2) 0.0221(5) Uani 1 1 d . . . H26 H 0.9260 1.0632 0.1111 0.027 Uiso 1 1 calc R . . C27 C 0.8324(3) 1.2144(2) 0.1903(2) 0.0238(6) Uani 1 1 d . . . C28 C 0.7137(3) 1.2602(3) 0.2626(2) 0.0249(6) Uani 1 1 d . . . C29 C 0.6894(3) 1.3683(3) 0.2934(3) 0.0311(6) Uani 1 1 d . . . H29 H 0.6095 1.3991 0.3430 0.037 Uiso 1 1 calc R . . C30 C 0.7841(3) 1.4310(3) 0.2503(3) 0.0314(6) Uani 1 1 d . . . H30 H 0.7660 1.5072 0.2687 0.038 Uiso 1 1 calc R . . C31 C 0.9044(3) 1.3876(3) 0.1817(2) 0.0283(6) Uani 1 1 d . . . C32 C 0.9269(3) 1.2774(2) 0.1515(2) 0.0236(6) Uani 1 1 d . . . C33 C 1.1340(3) 1.1507(4) 0.1435(3) 0.0411(8) Uani 1 1 d . . . H33C H 1.1407 1.1910 0.1971 0.062 Uiso 1 1 calc R . . H33B H 1.2184 1.1285 0.0905 0.062 Uiso 1 1 calc R . . H33A H 1.1043 1.0774 0.1862 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0580(16) 0.0539(15) 0.0328(12) 0.0013(11) -0.0207(12) -0.0304(13) O2 0.0362(12) 0.0420(13) 0.0327(12) -0.0041(10) -0.0092(10) -0.0176(10) O3 0.0396(12) 0.0304(11) 0.0212(10) 0.0003(8) -0.0067(9) -0.0148(9) O4 0.0273(10) 0.0288(10) 0.0231(10) -0.0076(8) -0.0063(8) -0.0066(8) O5 0.0298(11) 0.0378(12) 0.0247(10) -0.0097(9) -0.0023(8) -0.0129(9) C1 0.056(2) 0.068(3) 0.049(2) -0.034(2) -0.0193(18) -0.013(2) C2 0.055(2) 0.050(2) 0.049(2) -0.0043(17) -0.0137(18) -0.0310(18) C3 0.0430(18) 0.049(2) 0.0304(16) -0.0081(14) -0.0111(14) -0.0073(15) C4 0.0400(17) 0.0339(15) 0.0220(14) -0.0025(12) -0.0078(12) -0.0134(13) C5 0.0388(16) 0.0295(14) 0.0289(15) -0.0023(12) -0.0083(13) -0.0147(13) C6 0.0378(15) 0.0187(12) 0.0205(13) 0.0023(10) -0.0067(11) -0.0113(11) C7 0.0355(15) 0.0213(12) 0.0230(13) -0.0012(10) -0.0097(11) -0.0102(11) C8 0.0439(17) 0.0236(13) 0.0236(13) -0.0019(10) -0.0121(12) -0.0146(12) C9 0.0345(15) 0.0229(13) 0.0251(14) -0.0024(10) -0.0102(11) -0.0107(11) C10 0.0374(15) 0.0227(13) 0.0234(13) -0.0015(10) -0.0109(12) -0.0111(11) C11 0.0361(15) 0.0308(14) 0.0189(13) -0.0020(11) -0.0082(11) -0.0086(12) C12 0.0328(14) 0.0254(13) 0.0183(12) -0.0058(10) -0.0041(11) -0.0129(11) C13 0.0355(15) 0.0351(15) 0.0171(12) -0.0043(11) -0.0001(11) -0.0164(12) C14 0.0291(14) 0.0317(14) 0.0256(14) -0.0091(11) -0.0017(11) -0.0105(12) C15 0.0235(13) 0.0310(14) 0.0246(13) -0.0088(11) -0.0063(10) -0.0116(11) C16 0.0254(13) 0.0218(12) 0.0206(12) -0.0043(10) -0.0057(10) -0.0086(10) C17 0.0204(12) 0.0252(12) 0.0237(13) -0.0071(10) -0.0066(10) -0.0074(10) C18 0.0414(17) 0.0384(16) 0.0270(15) -0.0177(13) -0.0026(13) -0.0108(14) C19 0.0257(14) 0.0382(16) 0.0275(14) -0.0151(12) -0.0043(11) -0.0103(12) C20 0.0276(14) 0.0247(13) 0.0256(13) -0.0032(10) -0.0102(11) -0.0090(11) C21 0.0269(14) 0.0369(16) 0.0386(17) -0.0036(13) -0.0085(12) -0.0142(12) C22 0.0381(17) 0.0373(17) 0.0454(19) -0.0047(14) -0.0215(15) -0.0138(14) C23 0.0491(19) 0.0320(15) 0.0356(16) -0.0053(13) -0.0221(15) -0.0129(14) C24 0.0400(16) 0.0281(14) 0.0259(14) -0.0043(11) -0.0103(12) -0.0158(12) C25 0.0304(14) 0.0228(12) 0.0253(13) -0.0023(10) -0.0108(11) -0.0111(11) C26 0.0261(13) 0.0210(12) 0.0201(12) -0.0056(10) -0.0052(10) -0.0068(10) C27 0.0275(13) 0.0220(12) 0.0219(13) -0.0039(10) -0.0075(11) -0.0059(10) C28 0.0268(13) 0.0248(13) 0.0226(13) -0.0058(10) -0.0059(11) -0.0057(11) C29 0.0343(15) 0.0252(14) 0.0351(16) -0.0134(12) -0.0119(13) 0.0002(12) C30 0.0436(17) 0.0262(14) 0.0281(14) -0.0093(11) -0.0134(13) -0.0061(12) C31 0.0443(17) 0.0236(13) 0.0226(13) -0.0001(10) -0.0165(12) -0.0123(12) C32 0.0284(13) 0.0241(13) 0.0200(12) -0.0044(10) -0.0069(10) -0.0086(11) C33 0.0286(15) 0.052(2) 0.050(2) -0.0235(17) -0.0099(14) -0.0084(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C4 1.371(4) . ? O1 C1 1.421(5) . ? O2 C5 1.378(4) . ? O2 C2 1.440(5) . ? O3 C6 1.386(3) . ? O3 C3 1.437(4) . ? O4 C17 1.387(3) . ? O4 C18 1.437(4) . ? O5 C32 1.395(3) . ? O5 C33 1.421(4) . ? C1 H1C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 H2C 0.9800 . ? C2 H2B 0.9800 . ? C2 H2A 0.9800 . ? C3 H3A 0.9800 . ? C3 H3C 0.9800 . ? C3 H3B 0.9800 . ? C4 C10 1.394(4) . ? C4 C5 1.401(4) . ? C5 C6 1.395(4) . ? C6 C7 1.388(4) . ? C7 C9 1.399(4) . ? C7 C8 1.518(4) . ? C8 C31 1.501(4) 2_776 ? C8 H8B 0.9900 . ? C8 H8A 0.9900 . ? C9 C10 1.382(4) . ? C9 H9 0.9500 . ? C10 C11 1.513(4) . ? C11 C12 1.522(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.394(4) . ? C12 C17 1.402(4) . ? C13 C14 1.388(4) . ? C13 H13 0.9500 . ? C14 C15 1.377(4) . ? C14 H14 0.9500 . ? C15 C16 1.398(4) . ? C15 C19 1.522(4) . ? C16 C17 1.398(4) . ? C16 C26 1.524(4) . ? C18 H18C 0.9800 . ? C18 H18B 0.9800 . ? C18 H18A 0.9800 . ? C19 C28 1.520(4) . ? C19 C20 1.525(4) . ? C19 H19 1.0000 . ? C20 C21 1.378(4) . ? C20 C25 1.408(4) . ? C21 C22 1.394(5) . ? C21 H21 0.9500 . ? C22 C23 1.392(5) . ? C22 H22 0.9500 . ? C23 C24 1.381(5) . ? C23 H23 0.9500 . ? C24 C25 1.390(4) . ? C24 H24 0.9500 . ? C25 C26 1.527(4) . ? C26 C27 1.528(4) . ? C26 H26 1.0000 . ? C27 C32 1.387(4) . ? C27 C28 1.404(4) . ? C28 C29 1.380(4) . ? C29 C30 1.385(5) . ? C29 H29 0.9500 . ? C30 C31 1.388(5) . ? C30 H30 0.9500 . ? C31 C32 1.404(4) . ? C31 C8 1.501(4) 2_776 ? C33 H33C 0.9800 . ? C33 H33B 0.9800 . ? C33 H33A 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 O1 C1 116.5(3) . . ? C5 O2 C2 115.0(3) . . ? C6 O3 C3 113.8(2) . . ? C17 O4 C18 113.0(2) . . ? C32 O5 C33 112.6(2) . . ? O1 C1 H1C 109.5 . . ? O1 C1 H1A 109.5 . . ? H1C C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1C C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O2 C2 H2C 109.5 . . ? O2 C2 H2B 109.5 . . ? H2C C2 H2B 109.5 . . ? O2 C2 H2A 109.5 . . ? H2C C2 H2A 109.5 . . ? H2B C2 H2A 109.5 . . ? O3 C3 H3A 109.5 . . ? O3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? O3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? H3C C3 H3B 109.5 . . ? O1 C4 C10 118.7(3) . . ? O1 C4 C5 120.9(3) . . ? C10 C4 C5 120.3(3) . . ? O2 C5 C6 122.0(3) . . ? O2 C5 C4 118.4(3) . . ? C6 C5 C4 119.4(3) . . ? O3 C6 C7 118.5(3) . . ? O3 C6 C5 120.0(3) . . ? C7 C6 C5 121.4(3) . . ? C6 C7 C9 117.7(3) . . ? C6 C7 C8 118.9(2) . . ? C9 C7 C8 123.4(3) . . ? C31 C8 C7 116.1(2) 2_776 . ? C31 C8 H8B 108.3 2_776 . ? C7 C8 H8B 108.3 . . ? C31 C8 H8A 108.3 2_776 . ? C7 C8 H8A 108.3 . . ? H8B C8 H8A 107.4 . . ? C10 C9 C7 122.5(3) . . ? C10 C9 H9 118.7 . . ? C7 C9 H9 118.7 . . ? C9 C10 C4 118.8(3) . . ? C9 C10 C11 120.4(3) . . ? C4 C10 C11 120.8(3) . . ? C10 C11 C12 114.2(2) . . ? C10 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? C10 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C13 C12 C17 117.3(3) . . ? C13 C12 C11 122.9(3) . . ? C17 C12 C11 119.8(3) . . ? C14 C13 C12 122.4(3) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C15 C14 C13 119.5(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 119.8(3) . . ? C14 C15 C19 127.2(3) . . ? C16 C15 C19 113.0(2) . . ? C17 C16 C15 120.1(2) . . ? C17 C16 C26 126.2(2) . . ? C15 C16 C26 113.7(2) . . ? O4 C17 C16 120.1(2) . . ? O4 C17 C12 119.3(2) . . ? C16 C17 C12 120.6(3) . . ? O4 C18 H18C 109.5 . . ? O4 C18 H18B 109.5 . . ? H18C C18 H18B 109.5 . . ? O4 C18 H18A 109.5 . . ? H18C C18 H18A 109.5 . . ? H18B C18 H18A 109.5 . . ? C28 C19 C15 105.7(2) . . ? C28 C19 C20 106.2(2) . . ? C15 C19 C20 105.0(2) . . ? C28 C19 H19 113.1 . . ? C15 C19 H19 113.1 . . ? C20 C19 H19 113.1 . . ? C21 C20 C25 120.3(3) . . ? C21 C20 C19 126.4(3) . . ? C25 C20 C19 113.2(2) . . ? C20 C21 C22 118.9(3) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C23 C22 C21 120.9(3) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C24 C23 C22 120.4(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 119.1(3) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C20 120.4(3) . . ? C24 C25 C26 126.5(3) . . ? C20 C25 C26 113.0(2) . . ? C16 C26 C25 103.9(2) . . ? C16 C26 C27 105.1(2) . . ? C25 C26 C27 106.8(2) . . ? C16 C26 H26 113.4 . . ? C25 C26 H26 113.4 . . ? C27 C26 H26 113.4 . . ? C32 C27 C28 119.6(3) . . ? C32 C27 C26 126.9(3) . . ? C28 C27 C26 113.5(2) . . ? C29 C28 C27 120.5(3) . . ? C29 C28 C19 126.5(3) . . ? C27 C28 C19 112.9(2) . . ? C28 C29 C30 118.4(3) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? C29 C30 C31 123.1(3) . . ? C29 C30 H30 118.4 . . ? C31 C30 H30 118.4 . . ? C30 C31 C32 117.3(3) . . ? C30 C31 C8 121.1(3) . 2_776 ? C32 C31 C8 121.6(3) . 2_776 ? C27 C32 O5 119.5(2) . . ? C27 C32 C31 120.9(3) . . ? O5 C32 C31 119.7(3) . . ? O5 C33 H33C 109.5 . . ? O5 C33 H33B 109.5 . . ? H33C C33 H33B 109.5 . . ? O5 C33 H33A 109.5 . . ? H33C C33 H33A 109.5 . . ? H33B C33 H33A 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 O1 C4 C10 123.2(3) . . . . ? C1 O1 C4 C5 -60.5(4) . . . . ? C2 O2 C5 C6 -62.8(4) . . . . ? C2 O2 C5 C4 123.1(3) . . . . ? O1 C4 C5 O2 -1.2(5) . . . . ? C10 C4 C5 O2 175.0(3) . . . . ? O1 C4 C5 C6 -175.5(3) . . . . ? C10 C4 C5 C6 0.8(5) . . . . ? C3 O3 C6 C7 104.3(3) . . . . ? C3 O3 C6 C5 -78.3(4) . . . . ? O2 C5 C6 O3 8.6(5) . . . . ? C4 C5 C6 O3 -177.4(3) . . . . ? O2 C5 C6 C7 -174.1(3) . . . . ? C4 C5 C6 C7 -0.1(5) . . . . ? O3 C6 C7 C9 177.4(3) . . . . ? C5 C6 C7 C9 0.0(4) . . . . ? O3 C6 C7 C8 -2.7(4) . . . . ? C5 C6 C7 C8 180.0(3) . . . . ? C6 C7 C8 C31 -169.7(3) . . . 2_776 ? C9 C7 C8 C31 10.2(4) . . . 2_776 ? C6 C7 C9 C10 -0.7(4) . . . . ? C8 C7 C9 C10 179.4(3) . . . . ? C7 C9 C10 C4 1.4(5) . . . . ? C7 C9 C10 C11 -179.5(3) . . . . ? O1 C4 C10 C9 174.9(3) . . . . ? C5 C4 C10 C9 -1.4(5) . . . . ? O1 C4 C10 C11 -4.2(5) . . . . ? C5 C4 C10 C11 179.5(3) . . . . ? C9 C10 C11 C12 -104.8(3) . . . . ? C4 C10 C11 C12 74.3(4) . . . . ? C10 C11 C12 C13 -5.3(4) . . . . ? C10 C11 C12 C17 173.9(2) . . . . ? C17 C12 C13 C14 3.6(4) . . . . ? C11 C12 C13 C14 -177.2(3) . . . . ? C12 C13 C14 C15 -0.5(5) . . . . ? C13 C14 C15 C16 -3.6(4) . . . . ? C13 C14 C15 C19 176.2(3) . . . . ? C14 C15 C16 C17 4.5(4) . . . . ? C19 C15 C16 C17 -175.3(2) . . . . ? C14 C15 C16 C26 -177.7(2) . . . . ? C19 C15 C16 C26 2.4(3) . . . . ? C18 O4 C17 C16 -86.3(3) . . . . ? C18 O4 C17 C12 94.8(3) . . . . ? C15 C16 C17 O4 179.8(2) . . . . ? C26 C16 C17 O4 2.4(4) . . . . ? C15 C16 C17 C12 -1.4(4) . . . . ? C26 C16 C17 C12 -178.8(2) . . . . ? C13 C12 C17 O4 176.3(2) . . . . ? C11 C12 C17 O4 -3.0(4) . . . . ? C13 C12 C17 C16 -2.6(4) . . . . ? C11 C12 C17 C16 178.2(3) . . . . ? C14 C15 C19 C28 122.9(3) . . . . ? C16 C15 C19 C28 -57.3(3) . . . . ? C14 C15 C19 C20 -125.1(3) . . . . ? C16 C15 C19 C20 54.7(3) . . . . ? C28 C19 C20 C21 -127.8(3) . . . . ? C15 C19 C20 C21 120.5(3) . . . . ? C28 C19 C20 C25 55.4(3) . . . . ? C15 C19 C20 C25 -56.3(3) . . . . ? C25 C20 C21 C22 1.2(4) . . . . ? C19 C20 C21 C22 -175.4(3) . . . . ? C20 C21 C22 C23 -1.5(5) . . . . ? C21 C22 C23 C24 0.7(5) . . . . ? C22 C23 C24 C25 0.3(5) . . . . ? C23 C24 C25 C20 -0.6(4) . . . . ? C23 C24 C25 C26 175.5(3) . . . . ? C21 C20 C25 C24 -0.2(4) . . . . ? C19 C20 C25 C24 176.8(3) . . . . ? C21 C20 C25 C26 -176.8(3) . . . . ? C19 C20 C25 C26 0.2(3) . . . . ? C17 C16 C26 C25 119.4(3) . . . . ? C15 C16 C26 C25 -58.2(3) . . . . ? C17 C16 C26 C27 -128.5(3) . . . . ? C15 C16 C26 C27 53.9(3) . . . . ? C24 C25 C26 C16 -120.1(3) . . . . ? C20 C25 C26 C16 56.3(3) . . . . ? C24 C25 C26 C27 129.1(3) . . . . ? C20 C25 C26 C27 -54.5(3) . . . . ? C16 C26 C27 C32 122.7(3) . . . . ? C25 C26 C27 C32 -127.3(3) . . . . ? C16 C26 C27 C28 -56.8(3) . . . . ? C25 C26 C27 C28 53.2(3) . . . . ? C32 C27 C28 C29 1.2(4) . . . . ? C26 C27 C28 C29 -179.2(3) . . . . ? C32 C27 C28 C19 -177.0(2) . . . . ? C26 C27 C28 C19 2.5(3) . . . . ? C15 C19 C28 C29 -123.8(3) . . . . ? C20 C19 C28 C29 124.9(3) . . . . ? C15 C19 C28 C27 54.3(3) . . . . ? C20 C19 C28 C27 -56.9(3) . . . . ? C27 C28 C29 C30 0.8(4) . . . . ? C19 C28 C29 C30 178.8(3) . . . . ? C28 C29 C30 C31 -2.9(5) . . . . ? C29 C30 C31 C32 2.8(4) . . . . ? C29 C30 C31 C8 -176.9(3) . . . 2_776 ? C28 C27 C32 O5 179.3(2) . . . . ? C26 C27 C32 O5 -0.3(4) . . . . ? C28 C27 C32 C31 -1.2(4) . . . . ? C26 C27 C32 C31 179.2(3) . . . . ? C33 O5 C32 C27 -88.8(3) . . . . ? C33 O5 C32 C31 91.7(3) . . . . ? C30 C31 C32 C27 -0.7(4) . . . . ? C8 C31 C32 C27 179.0(3) 2_776 . . . ? C30 C31 C32 O5 178.8(2) . . . . ? C8 C31 C32 O5 -1.5(4) 2_776 . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.687 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.118 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 344 144 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 931897' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a3 #TrackingRef 'web_deposit_cif_file_3_Taoxie_1364731106.a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H58 Br2 Cl4 O8' _chemical_formula_weight 1280.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.493(2) _cell_length_b 11.851(2) _cell_length_c 12.708(3) _cell_angle_alpha 71.48(3) _cell_angle_beta 71.12(3) _cell_angle_gamma 72.93(3) _cell_volume 1517.4(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5204 _cell_measurement_theta_min 1.7474 _cell_measurement_theta_max 27.4725 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 1.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5208 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007HF + CCD (Saturn724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16886 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5342 _reflns_number_gt 4320 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1487P)^2^+2.0855P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5342 _refine_ls_number_parameters 440 _refine_ls_number_restraints 344 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0920 _refine_ls_wR_factor_ref 0.2809 _refine_ls_wR_factor_gt 0.2566 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.91208(13) 0.55450(13) 0.19926(12) 0.0503(6) Uani 0.436(2) 1 d PDU A 1 O1 O 0.8124(9) 0.4052(8) 0.4427(8) 0.0457(17) Uani 0.436(2) 1 d PDU A 1 O2 O 0.7266(15) 0.5629(11) 0.0692(10) 0.039(2) Uani 0.436(2) 1 d PDU A 1 C1 C 0.7673(11) 0.4892(11) 0.2557(10) 0.035(2) Uani 0.436(2) 1 d PDU A 1 C2 C 0.7308(11) 0.4241(12) 0.3713(10) 0.038(2) Uani 0.436(2) 1 d PDU A 1 C6 C 0.6954(13) 0.4988(14) 0.1843(11) 0.034(2) Uani 0.436(2) 1 d PDU A 1 C7 C 0.8203(15) 0.4974(13) -0.0064(12) 0.046(3) Uani 0.436(2) 1 d PDU A 1 H7B H 0.8482 0.5540 -0.0799 0.069 Uiso 0.436(2) 1 calc PR A 1 H7A H 0.7855 0.4378 -0.0187 0.069 Uiso 0.436(2) 1 calc PR A 1 H7C H 0.8920 0.4550 0.0271 0.069 Uiso 0.436(2) 1 calc PR A 1 C8 C 0.7961(15) 0.5048(12) 0.4877(12) 0.052(3) Uani 0.436(2) 1 d PDU A 1 H8C H 0.8759 0.5052 0.5000 0.078 Uiso 0.436(2) 1 calc PR A 1 H8B H 0.7318 0.4976 0.5610 0.078 Uiso 0.436(2) 1 calc PR A 1 H8A H 0.7692 0.5808 0.4336 0.078 Uiso 0.436(2) 1 calc PR A 1 Br1A Br 0.83247(12) 0.63041(11) 0.25751(10) 0.0585(5) Uani 0.564(2) 1 d PDU A 2 O1A O 0.7271(7) 0.4689(6) 0.4942(6) 0.0435(14) Uani 0.564(2) 1 d PDU A 2 O2A O 0.7089(10) 0.5894(8) 0.0964(7) 0.0350(19) Uani 0.564(2) 1 d PDU A 2 C1A C 0.7245(9) 0.5238(8) 0.2937(8) 0.0342(18) Uani 0.564(2) 1 d PDU A 2 C2A C 0.6880(10) 0.4575(9) 0.4047(8) 0.0367(18) Uani 0.564(2) 1 d PDU A 2 C6A C 0.6772(11) 0.5174(10) 0.2086(9) 0.034(2) Uani 0.564(2) 1 d PDU A 2 C7A C 0.8203(11) 0.5349(10) 0.0278(9) 0.045(2) Uani 0.564(2) 1 d PDU A 2 H7AB H 0.8480 0.5955 -0.0427 0.067 Uiso 0.564(2) 1 calc PR A 2 H7AA H 0.8050 0.4678 0.0082 0.067 Uiso 0.564(2) 1 calc PR A 2 H7AC H 0.8857 0.5033 0.0700 0.067 Uiso 0.564(2) 1 calc PR A 2 C8A C 0.8532(9) 0.4073(10) 0.4972(10) 0.050(2) Uani 0.564(2) 1 d PDU A 2 H8AB H 0.9083 0.4223 0.4194 0.075 Uiso 0.564(2) 1 calc PR A 2 H8AA H 0.8569 0.3196 0.5278 0.075 Uiso 0.564(2) 1 calc PR A 2 H8AC H 0.8810 0.4374 0.5464 0.075 Uiso 0.564(2) 1 calc PR A 2 Cl1 Cl 0.0635(3) 0.1533(4) 0.6741(3) 0.1351(13) Uani 1 1 d DU B 1 Cl2 Cl -0.1578(2) 0.2600(2) 0.82337(18) 0.0795(6) Uani 1 1 d DU B 1 O3 O 0.5477(3) 0.2333(3) 0.0781(3) 0.0412(9) Uani 1 1 d . . . O4 O 0.4950(3) -0.1509(3) 0.2330(3) 0.0372(8) Uani 1 1 d . . . C3 C 0.6121(6) 0.3807(5) 0.4263(5) 0.0448(12) Uani 1 1 d DU . . C4 C 0.5542(5) 0.3842(4) 0.3458(4) 0.0379(12) Uani 1 1 d . A . H4 H 0.4870 0.3431 0.3697 0.045 Uiso 1 1 calc R . . C5 C 0.5896(5) 0.4457(4) 0.2302(4) 0.0340(11) Uani 1 1 d DU . . C9 C 0.5250(6) 0.4539(5) 0.1399(5) 0.0442(13) Uani 1 1 d . A . H9B H 0.4897 0.5407 0.1086 0.053 Uiso 1 1 calc R . . H9A H 0.5890 0.4228 0.0761 0.053 Uiso 1 1 calc R . . C10 C 0.4225(6) 0.3858(5) 0.1821(5) 0.0427(13) Uani 1 1 d . . . C11 C 0.4363(5) 0.2770(4) 0.1521(4) 0.0354(11) Uani 1 1 d . A . C12 C 0.6350(6) 0.1476(7) 0.1380(6) 0.0571(16) Uani 1 1 d . . . H12B H 0.7113 0.1183 0.0827 0.086 Uiso 1 1 calc R . . H12A H 0.5972 0.0787 0.1882 0.086 Uiso 1 1 calc R . . H12C H 0.6566 0.1868 0.1843 0.086 Uiso 1 1 calc R . . C13 C 0.3379(5) 0.2147(4) 0.1925(4) 0.0309(10) Uani 1 1 d . . . C14 C 0.2278(5) 0.2567(4) 0.2671(4) 0.0340(11) Uani 1 1 d . A . C15 C 0.2096(6) 0.3634(5) 0.2994(5) 0.0475(14) Uani 1 1 d . . . H15 H 0.1330 0.3923 0.3500 0.057 Uiso 1 1 calc R A . C16 C 0.3057(6) 0.4264(5) 0.2563(5) 0.0489(14) Uani 1 1 d . A . H16 H 0.2930 0.5002 0.2771 0.059 Uiso 1 1 calc R . . C17 C 0.3386(5) 0.0983(4) 0.1645(4) 0.0296(10) Uani 1 1 d . A . H17 H 0.4182 0.0694 0.1093 0.035 Uiso 1 1 calc R . . C18 C 0.3128(4) 0.0052(4) 0.2792(4) 0.0270(10) Uani 1 1 d . . . C19 C 0.3839(4) -0.1082(4) 0.3090(4) 0.0293(10) Uani 1 1 d . A . C20 C 0.4712(6) -0.2014(5) 0.1554(5) 0.0450(13) Uani 1 1 d . . . H20A H 0.4172 -0.1386 0.1100 0.068 Uiso 1 1 calc R . . H20B H 0.4291 -0.2693 0.1991 0.068 Uiso 1 1 calc R . . H20C H 0.5511 -0.2310 0.1040 0.068 Uiso 1 1 calc R . . C21 C 0.3486(5) -0.1844(4) 0.4199(4) 0.0357(11) Uani 1 1 d . . . C22 C 0.4287(6) -0.3111(5) 0.4514(5) 0.0482(14) Uani 1 1 d . . . H22A H 0.4279 -0.3589 0.4005 0.058 Uiso 1 1 calc R . . H22B H 0.5166 -0.3038 0.4362 0.058 Uiso 1 1 calc R . . C23 C 0.2417(5) -0.1393(5) 0.4962(4) 0.0379(12) Uani 1 1 d . A . H23 H 0.2178 -0.1887 0.5715 0.045 Uiso 1 1 calc R . . C24 C 0.1679(5) -0.0235(5) 0.4660(4) 0.0378(12) Uani 1 1 d . . . H24 H 0.0951 0.0055 0.5202 0.045 Uiso 1 1 calc R A . C25 C 0.2017(5) 0.0488(4) 0.3566(4) 0.0320(10) Uani 1 1 d . A . C26 C 0.1317(5) 0.1741(5) 0.3083(4) 0.0350(11) Uani 1 1 d . . . H26 H 0.0523 0.2035 0.3635 0.042 Uiso 1 1 calc R A . C27 C 0.1109(5) 0.1686(5) 0.1971(4) 0.0360(11) Uani 1 1 d . A . C28 C 0.2216(5) 0.1255(4) 0.1204(4) 0.0319(10) Uani 1 1 d . . . C29 C 0.2188(6) 0.1105(5) 0.0174(5) 0.0425(13) Uani 1 1 d . A . H29 H 0.2942 0.0831 -0.0354 0.051 Uiso 1 1 calc R . . C30 C 0.1013(6) 0.1371(6) -0.0065(5) 0.0512(15) Uani 1 1 d . . . H30 H 0.0979 0.1272 -0.0767 0.061 Uiso 1 1 calc R A . C31 C -0.0085(6) 0.1768(5) 0.0680(5) 0.0478(14) Uani 1 1 d . A . H31 H -0.0868 0.1926 0.0500 0.057 Uiso 1 1 calc R . . C32 C -0.0049(5) 0.1942(5) 0.1722(5) 0.0435(13) Uani 1 1 d . . . H32 H -0.0803 0.2229 0.2242 0.052 Uiso 1 1 calc R A . C34 C -0.0876(8) 0.1442(8) 0.7528(8) 0.087(2) Uani 1 1 d DU . . H34B H -0.0865 0.0646 0.8098 0.104 Uiso 1 1 calc R B 1 H34A H -0.1381 0.1486 0.7010 0.104 Uiso 1 1 calc R B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0476(9) 0.0599(10) 0.0470(9) 0.0018(7) -0.0169(6) -0.0273(7) O1 0.053(4) 0.051(3) 0.042(3) -0.009(3) -0.021(3) -0.016(3) O2 0.046(4) 0.031(4) 0.032(4) 0.003(3) -0.009(4) -0.012(3) C1 0.042(4) 0.034(4) 0.034(4) -0.008(3) -0.013(4) -0.010(4) C2 0.045(4) 0.038(4) 0.039(4) -0.006(3) -0.020(3) -0.013(3) C6 0.042(4) 0.029(4) 0.029(4) 0.001(3) -0.011(3) -0.010(3) C7 0.052(5) 0.043(5) 0.035(5) -0.007(4) -0.005(4) -0.006(5) C8 0.058(5) 0.057(5) 0.049(4) -0.016(4) -0.020(4) -0.011(4) Br1A 0.0771(9) 0.0594(8) 0.0543(7) 0.0058(5) -0.0271(6) -0.0471(7) O1A 0.052(3) 0.050(3) 0.040(3) -0.015(3) -0.019(3) -0.016(3) O2A 0.041(3) 0.032(4) 0.025(3) 0.003(3) -0.005(3) -0.013(3) C1A 0.040(4) 0.035(3) 0.033(3) -0.007(3) -0.012(3) -0.014(3) C2A 0.049(4) 0.036(3) 0.033(3) -0.008(3) -0.018(3) -0.013(3) C6A 0.044(3) 0.029(3) 0.029(4) 0.001(3) -0.013(3) -0.013(3) C7A 0.051(4) 0.038(4) 0.035(4) -0.002(3) -0.003(4) -0.010(4) C8A 0.054(4) 0.058(4) 0.048(4) -0.013(4) -0.024(4) -0.014(4) Cl1 0.112(2) 0.191(3) 0.142(2) -0.109(2) 0.0091(18) -0.063(2) Cl2 0.0857(13) 0.0856(13) 0.0786(13) -0.0222(10) -0.0370(11) -0.0147(11) O3 0.050(2) 0.053(2) 0.0253(17) -0.0038(16) -0.0047(16) -0.0298(18) O4 0.043(2) 0.0391(18) 0.0337(18) -0.0099(15) -0.0132(15) -0.0105(16) C3 0.062(3) 0.035(2) 0.042(3) 0.003(2) -0.026(2) -0.017(2) C4 0.052(3) 0.027(2) 0.036(3) 0.002(2) -0.014(2) -0.018(2) C5 0.049(3) 0.027(2) 0.032(2) -0.0005(18) -0.016(2) -0.018(2) C9 0.071(4) 0.040(3) 0.034(3) -0.002(2) -0.021(3) -0.030(3) C10 0.061(3) 0.037(3) 0.042(3) -0.002(2) -0.027(3) -0.020(3) C11 0.049(3) 0.035(3) 0.027(2) 0.001(2) -0.021(2) -0.014(2) C12 0.044(3) 0.079(4) 0.058(4) -0.028(3) -0.011(3) -0.018(3) C13 0.041(3) 0.031(2) 0.026(2) 0.0036(19) -0.021(2) -0.013(2) C14 0.039(3) 0.033(2) 0.031(2) 0.000(2) -0.014(2) -0.013(2) C15 0.047(3) 0.046(3) 0.053(3) -0.016(3) -0.012(3) -0.012(3) C16 0.061(4) 0.036(3) 0.056(4) -0.011(3) -0.023(3) -0.010(3) C17 0.035(2) 0.034(2) 0.024(2) -0.0004(19) -0.0140(19) -0.015(2) C18 0.033(2) 0.031(2) 0.024(2) -0.0039(18) -0.0115(19) -0.016(2) C19 0.036(2) 0.035(2) 0.025(2) -0.0066(19) -0.011(2) -0.017(2) C20 0.058(3) 0.048(3) 0.036(3) -0.021(2) -0.010(3) -0.011(3) C21 0.050(3) 0.037(3) 0.029(2) -0.006(2) -0.018(2) -0.015(2) C22 0.080(4) 0.033(3) 0.032(3) 0.002(2) -0.026(3) -0.012(3) C23 0.057(3) 0.038(3) 0.022(2) 0.003(2) -0.011(2) -0.025(2) C24 0.043(3) 0.050(3) 0.028(2) -0.010(2) -0.006(2) -0.026(2) C25 0.036(3) 0.040(3) 0.029(2) -0.008(2) -0.012(2) -0.019(2) C26 0.036(3) 0.040(3) 0.032(3) -0.010(2) -0.009(2) -0.010(2) C27 0.040(3) 0.038(3) 0.035(3) 0.000(2) -0.018(2) -0.017(2) C28 0.038(3) 0.030(2) 0.031(2) 0.0017(19) -0.015(2) -0.014(2) C29 0.053(3) 0.045(3) 0.038(3) 0.002(2) -0.025(3) -0.020(3) C30 0.072(4) 0.058(3) 0.036(3) 0.007(3) -0.035(3) -0.030(3) C31 0.045(3) 0.053(3) 0.050(3) 0.006(3) -0.031(3) -0.016(3) C32 0.047(3) 0.041(3) 0.048(3) 0.001(2) -0.026(3) -0.015(2) C34 0.093(5) 0.083(5) 0.101(5) -0.035(4) -0.022(4) -0.033(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C1 1.875(11) . ? O1 C8 1.409(13) . ? O1 C2 1.432(12) . ? O2 C6 1.400(13) . ? O2 C7 1.413(14) . ? C1 C6 1.373(14) . ? C1 C2 1.413(13) . ? C2 C3 1.477(12) . ? C6 C5 1.404(13) . ? C7 H7B 0.9800 . ? C7 H7A 0.9800 . ? C7 H7C 0.9800 . ? C8 H8C 0.9800 . ? C8 H8B 0.9800 . ? C8 H8A 0.9800 . ? Br1A C1A 1.878(8) . ? O1A C2A 1.406(10) . ? O1A C8A 1.425(11) . ? O2A C7A 1.402(12) . ? O2A C6A 1.403(11) . ? C1A C2A 1.374(11) . ? C1A C6A 1.389(12) . ? C2A C3 1.349(10) . ? C6A C5 1.409(11) . ? C7A H7AB 0.9800 . ? C7A H7AA 0.9800 . ? C7A H7AC 0.9800 . ? C8A H8AB 0.9800 . ? C8A H8AA 0.9800 . ? C8A H8AC 0.9800 . ? Cl1 C34 1.716(9) . ? Cl2 C34 1.733(8) . ? O3 C11 1.390(6) . ? O3 C12 1.422(8) . ? O4 C19 1.397(6) . ? O4 C20 1.432(6) . ? C3 C4 1.373(7) . ? C3 C22 1.501(7) 2_656 ? C4 C5 1.401(7) . ? C4 H4 0.9500 . ? C5 C9 1.522(7) . ? C9 C10 1.483(8) . ? C9 H9B 0.9900 . ? C9 H9A 0.9900 . ? C10 C11 1.409(7) . ? C10 C16 1.418(8) . ? C11 C13 1.401(7) . ? C12 H12B 0.9800 . ? C12 H12A 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.379(7) . ? C13 C17 1.527(6) . ? C14 C15 1.389(7) . ? C14 C26 1.545(7) . ? C15 C16 1.383(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.523(6) . ? C17 C28 1.530(6) . ? C17 H17 1.0000 . ? C18 C19 1.360(7) . ? C18 C25 1.409(7) . ? C19 C21 1.415(7) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.381(7) . ? C21 C22 1.519(7) . ? C22 C3 1.501(7) 2_656 ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.394(8) . ? C23 H23 0.9500 . ? C24 C25 1.381(7) . ? C24 H24 0.9500 . ? C25 C26 1.507(7) . ? C26 C27 1.531(7) . ? C26 H26 1.0000 . ? C27 C32 1.392(7) . ? C27 C28 1.400(7) . ? C28 C29 1.388(7) . ? C29 C30 1.404(8) . ? C29 H29 0.9500 . ? C30 C31 1.368(9) . ? C30 H30 0.9500 . ? C31 C32 1.419(8) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C34 H34B 0.9900 . ? C34 H34A 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 O1 C2 114.5(10) . . ? C6 O2 C7 116.0(11) . . ? C6 C1 C2 117.5(10) . . ? C6 C1 Br1 120.7(8) . . ? C2 C1 Br1 121.8(8) . . ? C1 C2 O1 117.1(9) . . ? C1 C2 C3 125.5(9) . . ? O1 C2 C3 117.2(9) . . ? C1 C6 O2 119.9(12) . . ? C1 C6 C5 118.5(10) . . ? O2 C6 C5 121.6(12) . . ? C2A O1A C8A 114.6(8) . . ? C7A O2A C6A 113.1(8) . . ? C2A C1A C6A 120.5(8) . . ? C2A C1A Br1A 120.1(6) . . ? C6A C1A Br1A 119.4(7) . . ? C3 C2A C1A 118.1(7) . . ? C3 C2A O1A 120.2(7) . . ? C1A C2A O1A 121.7(8) . . ? C1A C6A O2A 120.8(9) . . ? C1A C6A C5 122.9(8) . . ? O2A C6A C5 116.1(9) . . ? O2A C7A H7AB 109.5 . . ? O2A C7A H7AA 109.5 . . ? H7AB C7A H7AA 109.5 . . ? O2A C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? O1A C8A H8AB 109.5 . . ? O1A C8A H8AA 109.5 . . ? H8AB C8A H8AA 109.5 . . ? O1A C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? H8AA C8A H8AC 109.5 . . ? C11 O3 C12 112.3(4) . . ? C19 O4 C20 111.8(4) . . ? C2A C3 C4 121.1(6) . . ? C2A C3 C2 26.5(5) . . ? C4 C3 C2 111.1(6) . . ? C2A C3 C22 117.1(6) . 2_656 ? C4 C3 C22 120.5(5) . 2_656 ? C2 C3 C22 126.6(6) . 2_656 ? C3 C4 C5 123.1(5) . . ? C3 C4 H4 118.4 . . ? C5 C4 H4 118.4 . . ? C4 C5 C6 122.7(7) . . ? C4 C5 C6A 113.1(6) . . ? C6 C5 C6A 16.5(8) . . ? C4 C5 C9 124.2(4) . . ? C6 C5 C9 112.9(7) . . ? C6A C5 C9 121.9(6) . . ? C10 C9 C5 114.7(4) . . ? C10 C9 H9B 108.6 . . ? C5 C9 H9B 108.6 . . ? C10 C9 H9A 108.6 . . ? C5 C9 H9A 108.6 . . ? H9B C9 H9A 107.6 . . ? C11 C10 C16 116.5(5) . . ? C11 C10 C9 122.0(5) . . ? C16 C10 C9 121.4(5) . . ? O3 C11 C13 119.6(4) . . ? O3 C11 C10 119.4(5) . . ? C13 C11 C10 121.0(5) . . ? O3 C12 H12B 109.5 . . ? O3 C12 H12A 109.5 . . ? H12B C12 H12A 109.5 . . ? O3 C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? C14 C13 C11 119.8(4) . . ? C14 C13 C17 113.6(4) . . ? C11 C13 C17 126.5(4) . . ? C13 C14 C15 121.4(5) . . ? C13 C14 C26 113.3(4) . . ? C15 C14 C26 125.3(5) . . ? C16 C15 C14 118.4(5) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? C15 C16 C10 122.8(5) . . ? C15 C16 H16 118.6 . . ? C10 C16 H16 118.6 . . ? C18 C17 C13 106.0(4) . . ? C18 C17 C28 105.0(4) . . ? C13 C17 C28 106.2(4) . . ? C18 C17 H17 113.0 . . ? C13 C17 H17 113.0 . . ? C28 C17 H17 113.0 . . ? C19 C18 C25 121.1(4) . . ? C19 C18 C17 126.8(4) . . ? C25 C18 C17 112.1(4) . . ? C18 C19 O4 121.2(4) . . ? C18 C19 C21 120.4(4) . . ? O4 C19 C21 118.4(4) . . ? O4 C20 H20A 109.5 . . ? O4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 C19 118.0(5) . . ? C23 C21 C22 122.4(5) . . ? C19 C21 C22 119.6(5) . . ? C3 C22 C21 115.1(5) 2_656 . ? C3 C22 H22A 108.5 2_656 . ? C21 C22 H22A 108.5 . . ? C3 C22 H22B 108.5 2_656 . ? C21 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? C21 C23 C24 122.0(5) . . ? C21 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C25 C24 C23 119.4(5) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C18 119.1(5) . . ? C24 C25 C26 126.6(5) . . ? C18 C25 C26 114.3(4) . . ? C25 C26 C27 106.0(4) . . ? C25 C26 C14 105.3(4) . . ? C27 C26 C14 104.0(4) . . ? C25 C26 H26 113.6 . . ? C27 C26 H26 113.6 . . ? C14 C26 H26 113.6 . . ? C32 C27 C28 120.2(5) . . ? C32 C27 C26 125.9(5) . . ? C28 C27 C26 113.7(4) . . ? C29 C28 C27 121.0(5) . . ? C29 C28 C17 126.4(5) . . ? C27 C28 C17 112.6(4) . . ? C28 C29 C30 118.0(5) . . ? C28 C29 H29 121.0 . . ? C30 C29 H29 121.0 . . ? C31 C30 C29 122.1(5) . . ? C31 C30 H30 118.9 . . ? C29 C30 H30 118.9 . . ? C30 C31 C32 119.6(5) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C27 C32 C31 118.9(5) . . ? C27 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? Cl1 C34 Cl2 112.0(5) . . ? Cl1 C34 H34B 109.2 . . ? Cl2 C34 H34B 109.2 . . ? Cl1 C34 H34A 109.2 . . ? Cl2 C34 H34A 109.2 . . ? H34B C34 H34A 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 O1 174.6(12) . . . . ? Br1 C1 C2 O1 -2.7(17) . . . . ? C6 C1 C2 C3 -9(2) . . . . ? Br1 C1 C2 C3 173.2(9) . . . . ? C8 O1 C2 C1 81.9(16) . . . . ? C8 O1 C2 C3 -94.3(13) . . . . ? C2 C1 C6 O2 179.6(12) . . . . ? Br1 C1 C6 O2 -3.0(19) . . . . ? C2 C1 C6 C5 1(2) . . . . ? Br1 C1 C6 C5 178.4(9) . . . . ? C7 O2 C6 C1 83.3(19) . . . . ? C7 O2 C6 C5 -98.2(17) . . . . ? C6A C1A C2A C3 4.3(15) . . . . ? Br1A C1A C2A C3 -178.9(7) . . . . ? C6A C1A C2A O1A -175.3(10) . . . . ? Br1A C1A C2A O1A 1.5(14) . . . . ? C8A O1A C2A C3 103.1(11) . . . . ? C8A O1A C2A C1A -77.3(12) . . . . ? C2A C1A C6A O2A 176.7(10) . . . . ? Br1A C1A C6A O2A -0.1(14) . . . . ? C2A C1A C6A C5 0.9(17) . . . . ? Br1A C1A C6A C5 -175.9(7) . . . . ? C7A O2A C6A C1A 87.3(13) . . . . ? C7A O2A C6A C5 -96.7(12) . . . . ? C1A C2A C3 C4 -11.8(13) . . . . ? O1A C2A C3 C4 167.8(7) . . . . ? C1A C2A C3 C2 62.9(14) . . . . ? O1A C2A C3 C2 -117.5(18) . . . . ? C1A C2A C3 C22 -178.8(8) . . . 2_656 ? O1A C2A C3 C22 0.8(12) . . . 2_656 ? C1 C2 C3 C2A -103(2) . . . . ? O1 C2 C3 C2A 73.2(15) . . . . ? C1 C2 C3 C4 14.9(16) . . . . ? O1 C2 C3 C4 -169.1(9) . . . . ? C1 C2 C3 C22 179.8(10) . . . 2_656 ? O1 C2 C3 C22 -4.2(15) . . . 2_656 ? C2A C3 C4 C5 14.6(10) . . . . ? C2 C3 C4 C5 -12.9(9) . . . . ? C22 C3 C4 C5 -178.8(5) 2_656 . . . ? C3 C4 C5 C6 6.5(11) . . . . ? C3 C4 C5 C6A -8.6(9) . . . . ? C3 C4 C5 C9 -178.3(5) . . . . ? C1 C6 C5 C4 0.4(17) . . . . ? O2 C6 C5 C4 -178.1(9) . . . . ? C1 C6 C5 C6A 59(3) . . . . ? O2 C6 C5 C6A -120(4) . . . . ? C1 C6 C5 C9 -175.2(11) . . . . ? O2 C6 C5 C9 6.3(16) . . . . ? C1A C6A C5 C4 1.1(13) . . . . ? O2A C6A C5 C4 -174.9(7) . . . . ? C1A C6A C5 C6 -128(4) . . . . ? O2A C6A C5 C6 56(3) . . . . ? C1A C6A C5 C9 171.0(9) . . . . ? O2A C6A C5 C9 -4.9(12) . . . . ? C4 C5 C9 C10 -2.8(8) . . . . ? C6 C5 C9 C10 172.8(8) . . . . ? C6A C5 C9 C10 -171.6(7) . . . . ? C5 C9 C10 C11 -107.5(6) . . . . ? C5 C9 C10 C16 71.8(7) . . . . ? C12 O3 C11 C13 -88.5(5) . . . . ? C12 O3 C11 C10 93.7(5) . . . . ? C16 C10 C11 O3 178.9(4) . . . . ? C9 C10 C11 O3 -1.8(7) . . . . ? C16 C10 C11 C13 1.1(7) . . . . ? C9 C10 C11 C13 -179.6(4) . . . . ? O3 C11 C13 C14 179.2(4) . . . . ? C10 C11 C13 C14 -3.1(7) . . . . ? O3 C11 C13 C17 0.5(7) . . . . ? C10 C11 C13 C17 178.3(4) . . . . ? C11 C13 C14 C15 2.9(7) . . . . ? C17 C13 C14 C15 -178.3(5) . . . . ? C11 C13 C14 C26 -177.0(4) . . . . ? C17 C13 C14 C26 1.8(5) . . . . ? C13 C14 C15 C16 -0.8(8) . . . . ? C26 C14 C15 C16 179.1(5) . . . . ? C14 C15 C16 C10 -1.1(9) . . . . ? C11 C10 C16 C15 1.0(8) . . . . ? C9 C10 C16 C15 -178.3(5) . . . . ? C14 C13 C17 C18 -56.7(5) . . . . ? C11 C13 C17 C18 122.0(5) . . . . ? C14 C13 C17 C28 54.6(5) . . . . ? C11 C13 C17 C28 -126.7(5) . . . . ? C13 C17 C18 C19 -126.0(5) . . . . ? C28 C17 C18 C19 121.8(5) . . . . ? C13 C17 C18 C25 54.4(5) . . . . ? C28 C17 C18 C25 -57.8(5) . . . . ? C25 C18 C19 O4 -179.1(4) . . . . ? C17 C18 C19 O4 1.4(7) . . . . ? C25 C18 C19 C21 -1.1(7) . . . . ? C17 C18 C19 C21 179.4(4) . . . . ? C20 O4 C19 C18 -84.5(5) . . . . ? C20 O4 C19 C21 97.5(5) . . . . ? C18 C19 C21 C23 -0.9(7) . . . . ? O4 C19 C21 C23 177.1(4) . . . . ? C18 C19 C21 C22 179.6(5) . . . . ? O4 C19 C21 C22 -2.3(7) . . . . ? C23 C21 C22 C3 -3.7(8) . . . 2_656 ? C19 C21 C22 C3 175.7(5) . . . 2_656 ? C19 C21 C23 C24 1.4(7) . . . . ? C22 C21 C23 C24 -179.2(5) . . . . ? C21 C23 C24 C25 0.3(7) . . . . ? C23 C24 C25 C18 -2.3(7) . . . . ? C23 C24 C25 C26 178.2(5) . . . . ? C19 C18 C25 C24 2.8(7) . . . . ? C17 C18 C25 C24 -177.6(4) . . . . ? C19 C18 C25 C26 -177.7(4) . . . . ? C17 C18 C25 C26 1.9(5) . . . . ? C24 C25 C26 C27 -126.8(5) . . . . ? C18 C25 C26 C27 53.7(5) . . . . ? C24 C25 C26 C14 123.4(5) . . . . ? C18 C25 C26 C14 -56.0(5) . . . . ? C13 C14 C26 C25 54.0(5) . . . . ? C15 C14 C26 C25 -125.9(5) . . . . ? C13 C14 C26 C27 -57.2(5) . . . . ? C15 C14 C26 C27 122.9(5) . . . . ? C25 C26 C27 C32 122.0(5) . . . . ? C14 C26 C27 C32 -127.3(5) . . . . ? C25 C26 C27 C28 -53.6(6) . . . . ? C14 C26 C27 C28 57.1(5) . . . . ? C32 C27 C28 C29 1.7(7) . . . . ? C26 C27 C28 C29 177.6(4) . . . . ? C32 C27 C28 C17 -178.0(4) . . . . ? C26 C27 C28 C17 -2.1(6) . . . . ? C18 C17 C28 C29 -121.9(5) . . . . ? C13 C17 C28 C29 126.1(5) . . . . ? C18 C17 C28 C27 57.8(5) . . . . ? C13 C17 C28 C27 -54.2(5) . . . . ? C27 C28 C29 C30 -1.5(8) . . . . ? C17 C28 C29 C30 178.1(5) . . . . ? C28 C29 C30 C31 0.1(8) . . . . ? C29 C30 C31 C32 1.2(9) . . . . ? C28 C27 C32 C31 -0.5(8) . . . . ? C26 C27 C32 C31 -175.8(5) . . . . ? C30 C31 C32 C27 -0.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.202 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.139 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.500 113 43 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 931898' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a #TrackingRef 'web_deposit_cif_file_0_Taoxie_1364836116.a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H57 Cl15 O8' _chemical_formula_weight 1521.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.999(4) _cell_length_b 19.134(4) _cell_length_c 33.115(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.09(3) _cell_angle_gamma 90.00 _cell_volume 13800(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 29888 _cell_measurement_theta_min 0.9349 _cell_measurement_theta_max 24.9793 _exptl_crystal_description plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.59 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6224 _exptl_absorpt_coefficient_mu 0.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6712 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79446 _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 24.97 _reflns_number_total 24153 _reflns_number_gt 20699 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0946P)^2^+91.9265P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24153 _refine_ls_number_parameters 1621 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1855 _refine_ls_R_factor_gt 0.1658 _refine_ls_wR_factor_ref 0.3536 _refine_ls_wR_factor_gt 0.3414 _refine_ls_goodness_of_fit_ref 1.303 _refine_ls_restrained_S_all 1.303 _refine_ls_shift/su_max 1.064 _refine_ls_shift/su_mean 0.007 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl15 Cl 0.04006(11) 0.20394(13) 0.31235(8) 0.0474(6) Uani 1 1 d . . . Cl9 Cl 0.46098(11) 0.73667(13) 0.18790(8) 0.0468(6) Uani 1 1 d . . . Cl12 Cl 0.38672(11) 0.58741(14) 0.33769(8) 0.0497(6) Uani 1 1 d . . . Cl6 Cl 0.10954(11) 0.35493(14) 0.15890(8) 0.0509(6) Uani 1 1 d . . . Cl8 Cl 0.48210(12) 0.58806(13) 0.18410(9) 0.0522(7) Uani 1 1 d . . . Cl14 Cl 0.01493(12) 0.35229(13) 0.31420(9) 0.0529(7) Uani 1 1 d . . . Cl11 Cl 0.27759(13) 0.50310(17) 0.31873(9) 0.0636(8) Uani 1 1 d . . . Cl5 Cl 0.21778(12) 0.44054(16) 0.17602(10) 0.0625(8) Uani 1 1 d . . . Cl3 Cl 0.76623(15) 0.90953(16) -0.15130(11) 0.0716(9) Uani 1 1 d . . . Cl18 Cl 0.26796(15) 0.85238(17) 0.34871(12) 0.0778(9) Uani 1 1 d . . . Cl10 Cl 0.31776(14) 0.5471(2) 0.40158(9) 0.0774(10) Uani 1 1 d . . . Cl2 Cl 0.76512(15) 0.76070(17) -0.16264(13) 0.0853(11) Uani 1 1 d . . . Cl4 Cl 0.17580(15) 0.3956(2) 0.09355(9) 0.0813(11) Uani 1 1 d . . . Cl7 Cl 0.5154(2) 0.6785(2) 0.12049(11) 0.0942(12) Uani 1 1 d . . . Cl13 Cl -0.0147(2) 0.2628(2) 0.37903(12) 0.0961(12) Uani 1 1 d . . . Cl17 Cl 0.26644(17) 0.7051(2) 0.33352(15) 0.1033(14) Uani 1 1 d . . . O1 O 1.0908(2) 0.9939(3) 0.22495(16) 0.0317(13) Uani 1 1 d . . . O2 O 0.9031(2) 1.0233(3) 0.15337(16) 0.0293(13) Uani 1 1 d . . . O3 O 0.8475(3) 0.5719(3) 0.15228(17) 0.0344(14) Uani 1 1 d . . . O4 O 1.0359(3) 0.5468(3) 0.21882(16) 0.0314(13) Uani 1 1 d . . . O5 O 1.0457(3) 0.6472(3) 0.27629(17) 0.0322(13) Uani 1 1 d . . . H5 H 1.0435 0.6177 0.2574 0.039 Uiso 1 1 d R . . O6 O 1.0788(2) 0.8904(3) 0.28281(17) 0.0302(13) Uani 1 1 d . . . H6 H 1.0779 0.9214 0.2648 0.036 Uiso 1 1 d R . . O7 O 0.8436(3) 0.9226(3) 0.19328(17) 0.0351(14) Uani 1 1 d . . . H7 H 0.8526 0.9545 0.1777 0.042 Uiso 1 1 d R . . O8 O 0.8010(3) 0.6812(3) 0.19117(17) 0.0354(14) Uani 1 1 d . . . H8 H 0.8067 0.6443 0.1785 0.042 Uiso 1 1 d R . . O9 O 0.3500(2) 0.8704(3) 0.14944(17) 0.0302(13) Uani 1 1 d . . . O10 O 0.5382(2) 0.8947(3) 0.22068(16) 0.0296(13) Uani 1 1 d . . . O11 O 0.4015(2) 0.4182(3) 0.14955(17) 0.0313(13) Uani 1 1 d . . . O12 O 0.5870(3) 0.4470(3) 0.22315(16) 0.0300(13) Uani 1 1 d . . . O13 O 0.5730(3) 0.5488(3) 0.28168(18) 0.0365(14) Uani 1 1 d . . . H13 H 0.5712 0.5155 0.2650 0.044 Uiso 1 1 d R . . O14 O 0.5452(2) 0.7937(3) 0.27795(16) 0.0322(13) Uani 1 1 d . . . H14 H 0.5500 0.8236 0.2601 0.039 Uiso 1 1 d R . . O15 O 0.3398(3) 0.5182(3) 0.18852(17) 0.0347(14) Uani 1 1 d . . . H15 H 0.3399 0.4819 0.1743 0.042 Uiso 1 1 d R . . O16 O 0.3022(3) 0.7604(3) 0.18708(17) 0.0347(14) Uani 1 1 d . . . H16 H 0.3074 0.7972 0.1742 0.042 Uiso 1 1 d R . . Cl1 Cl 0.6803(2) 0.8242(2) -0.11459(13) 0.1048(15) Uani 1 1 d . . . Cl21 Cl 0.66496(19) 0.9040(2) 0.01337(14) 0.0993(13) Uani 1 1 d . . . Cl16 Cl 0.1872(3) 0.7639(3) 0.38590(15) 0.146(2) Uani 1 1 d . . . Cl20 Cl 0.65553(18) 1.0439(2) -0.01838(13) 0.0979(13) Uani 1 1 d . . . Cl19 Cl 0.75232(19) 0.9538(3) -0.03623(16) 0.134(2) Uani 1 1 d . . . C40 C 0.8199(3) 0.8036(4) 0.1917(2) 0.0284(18) Uani 1 1 d . . . C42 C 1.1643(3) 0.7544(4) 0.2371(2) 0.0257(18) Uani 1 1 d . . . H42A H 1.1991 0.7494 0.2232 0.031 Uiso 1 1 calc R . . C44 C 0.9239(4) 0.9912(5) 0.1199(2) 0.033(2) Uani 1 1 d . . . C46 C 0.6094(3) 0.4754(4) 0.1892(2) 0.0267(18) Uani 1 1 d . . . C47 C 1.1127(4) 0.9653(4) 0.1904(2) 0.0256(17) Uani 1 1 d . . . C48 C 0.6525(4) 0.8195(4) 0.2348(2) 0.0263(17) Uani 1 1 d . . . H48A H 0.6430 0.8554 0.2545 0.032 Uiso 1 1 calc R . . H48B H 0.6976 0.8186 0.2351 0.032 Uiso 1 1 calc R . . C49 C 0.6183(4) 0.8364(5) 0.1186(3) 0.035(2) Uani 1 1 d . . . H49A H 0.6370 0.8239 0.0955 0.042 Uiso 1 1 calc R . . C50 C 0.3196(3) 0.6387(5) 0.1864(2) 0.0283(18) Uani 1 1 d . . . C51 C 0.9843(3) 0.9991(4) 0.1139(2) 0.0265(18) Uani 1 1 d . . . C52 C 0.6621(3) 0.6873(5) 0.2393(2) 0.032(2) Uani 1 1 d . . . H52A H 0.6975 0.6921 0.2261 0.039 Uiso 1 1 calc R . . C53 C 0.2956(3) 0.7004(5) 0.1220(2) 0.0265(18) Uani 1 1 d . . . C54 C 0.6309(4) 0.7481(4) 0.2477(2) 0.0280(19) Uani 1 1 d . . . C55 C 0.8255(4) 0.8653(5) 0.1693(2) 0.032(2) Uani 1 1 d . . . C56 C 1.0640(4) 0.7682(4) 0.2791(2) 0.0301(19) Uani 1 1 d . . . C57 C 1.1123(4) 0.6054(4) 0.1151(2) 0.0296(19) Uani 1 1 d . . . H57A H 1.1298 0.6180 0.0915 0.036 Uiso 1 1 calc R . . C59 C 0.2985(3) 0.6362(5) 0.1016(2) 0.0289(18) Uani 1 1 d . . . H59A H 0.2910 0.6358 0.0726 0.035 Uiso 1 1 calc R . . C60 C 0.4223(4) 0.4498(4) 0.1159(3) 0.0326(19) Uani 1 1 d . . . C61 C 0.7921(3) 0.7428(4) 0.1259(2) 0.0260(18) Uani 1 1 d . . . C62 C 1.1506(3) 0.9019(4) 0.1219(3) 0.0306(19) Uani 1 1 d . . . H62A H 1.1642 0.8806 0.0989 0.037 Uiso 1 1 calc R . . C63 C 1.1830(4) 0.8829(5) 0.2374(3) 0.0321(19) Uani 1 1 d . . . H63A H 1.2264 0.8690 0.2374 0.039 Uiso 1 1 calc R . . H63B H 1.1821 0.9197 0.2583 0.039 Uiso 1 1 calc R . . C64 C 0.5797(3) 0.7389(5) 0.2676(2) 0.0289(19) Uani 1 1 d . . . C65 C 1.1325(4) 0.6952(5) 0.2450(2) 0.032(2) Uani 1 1 d . . . C66 C 0.2854(4) 0.7676(4) 0.0966(2) 0.0293(18) Uani 1 1 d . . . H66A H 0.2599 0.7570 0.0702 0.035 Uiso 1 1 calc R . . H66B H 0.2630 0.8021 0.1112 0.035 Uiso 1 1 calc R . . C67 C 0.5095(3) 0.9690(4) 0.0760(2) 0.0266(18) Uani 1 1 d . . . C68 C 1.1581(4) 0.9131(4) 0.1956(3) 0.0291(18) Uani 1 1 d . . . C69 C 1.0866(4) 0.9855(4) 0.1511(2) 0.0298(18) Uani 1 1 d . . . C70 C 0.8711(4) 0.5938(5) 0.1173(3) 0.0306(19) Uani 1 1 d . . . C72 C 1.1479(3) 0.8219(4) 0.2485(2) 0.0223(17) Uani 1 1 d . . . C73 C 0.8175(4) 0.9356(5) 0.1025(2) 0.0314(19) Uani 1 1 d . . . H73A H 0.7903 0.9329 0.0760 0.038 Uiso 1 1 calc R . . H73B H 0.8036 0.9754 0.1180 0.038 Uiso 1 1 calc R . . C74 C 0.6484(4) 0.5410(5) 0.1219(3) 0.034(2) Uani 1 1 d . . . H74A H 0.6610 0.5638 0.0989 0.041 Uiso 1 1 calc R . . C75 C 0.9269(4) 0.5683(5) 0.1104(2) 0.0294(19) Uani 1 1 d . . . C76 C 0.3054(3) 0.6997(4) 0.1648(2) 0.0263(17) Uani 1 1 d . . . C77 C 1.1176(3) 0.6016(4) 0.1888(3) 0.0299(19) Uani 1 1 d . . . C78 C 0.4813(4) 0.9868(4) 0.1101(2) 0.0286(18) Uani 1 1 d . . . C79 C 0.6535(4) 0.5279(4) 0.1955(2) 0.0293(18) Uani 1 1 d . . . C80 C 0.5596(3) 0.6716(4) 0.2795(2) 0.0292(18) Uani 1 1 d . . . C81 C 1.0970(3) 0.8268(4) 0.2696(2) 0.0225(16) Uani 1 1 d . . . C82 C 0.5940(4) 0.6143(5) 0.2700(3) 0.037(2) Uani 1 1 d . . . C83 C 1.1505(4) 0.6219(5) 0.2309(3) 0.034(2) Uani 1 1 d . . . H83A H 1.1953 0.6207 0.2305 0.040 Uiso 1 1 calc R . . H83B H 1.1408 0.5868 0.2511 0.040 Uiso 1 1 calc R . . C84 C 0.8828(4) 0.9480(5) 0.0950(2) 0.036(2) Uani 1 1 d . . . C85 C 0.7799(3) 0.6760(5) 0.1014(2) 0.0308(19) Uani 1 1 d . . . H85A H 0.7525 0.6865 0.0758 0.037 Uiso 1 1 calc R . . H85B H 0.7584 0.6423 0.1172 0.037 Uiso 1 1 calc R . . C86 C 0.8125(3) 0.8672(5) 0.1265(3) 0.0304(19) Uani 1 1 d . . . C87 C 0.4658(4) 0.5149(5) 0.0503(3) 0.037(2) Uani 1 1 d . . . H87A H 0.4802 0.5365 0.0276 0.044 Uiso 1 1 calc R . . C88 C 0.4336(4) 0.8736(4) 0.1101(3) 0.0289(18) Uani 1 1 d . . . C89 C 0.8359(4) 0.8009(5) 0.2372(2) 0.038(2) Uani 1 1 d . . . H89A H 0.8292 0.7534 0.2468 0.057 Uiso 1 1 calc R . . H89B H 0.8097 0.8336 0.2497 0.057 Uiso 1 1 calc R . . H89C H 0.8790 0.8138 0.2449 0.057 Uiso 1 1 calc R . . C90 C 0.6798(4) 0.5547(4) 0.2376(2) 0.0291(18) Uani 1 1 d . . . H90A H 0.7237 0.5663 0.2380 0.035 Uiso 1 1 calc R . . H90B H 0.6769 0.5175 0.2581 0.035 Uiso 1 1 calc R . . C91 C 0.5358(4) 0.8906(4) 0.1485(3) 0.0320(19) Uani 1 1 d . . . C92 C 1.1061(3) 0.9537(5) 0.1172(2) 0.0290(18) Uani 1 1 d . . . C93 C 0.9524(4) 0.5891(4) 0.0753(2) 0.0282(18) Uani 1 1 d . . . C94 C 0.3324(4) 0.6381(5) 0.2326(3) 0.037(2) Uani 1 1 d . . . H94A H 0.3274 0.6854 0.2430 0.056 Uiso 1 1 calc R . . H94B H 0.3745 0.6220 0.2413 0.056 Uiso 1 1 calc R . . H94C H 0.3035 0.6064 0.2433 0.056 Uiso 1 1 calc R . . C95 C 0.5843(3) 0.4565(4) 0.1497(2) 0.0258(17) Uani 1 1 d . . . C96 C 0.9576(4) 0.3864(4) 0.1120(3) 0.0322(19) Uani 1 1 d . . . H96A H 0.9394 0.3728 0.1351 0.039 Uiso 1 1 calc R . . C97 C 0.3122(4) 0.5723(4) 0.1224(2) 0.0301(19) Uani 1 1 d . . . C98 C 0.7956(4) 0.8052(4) 0.1062(2) 0.0266(18) Uani 1 1 d . . . H98A H 0.7859 0.8062 0.0774 0.032 Uiso 1 1 calc R . . C99 C 0.8386(4) 0.6425(4) 0.0911(2) 0.0274(18) Uani 1 1 d . . . C100 C 0.3769(4) 0.8488(4) 0.1155(2) 0.0265(18) Uani 1 1 d . . . C101 C 1.0063(4) 0.7750(5) 0.3002(3) 0.037(2) Uani 1 1 d . . . H10A H 1.0003 0.8241 0.3071 0.056 Uiso 1 1 calc R . . H10B H 1.0113 0.7468 0.3251 0.056 Uiso 1 1 calc R . . H10C H 0.9704 0.7585 0.2817 0.056 Uiso 1 1 calc R . . C102 C 0.4834(4) 0.4414(4) 0.1092(3) 0.0292(18) Uani 1 1 d . . . C103 C 1.0016(4) 0.4765(5) 0.0726(2) 0.034(2) Uani 1 1 d . . . C104 C 0.5693(4) 0.2793(5) 0.1160(3) 0.035(2) Uani 1 1 d . . . H10D H 0.5555 0.2576 0.1388 0.043 Uiso 1 1 calc R . . C105 C 0.3816(3) 0.4922(4) 0.0898(2) 0.0257(17) Uani 1 1 d . . . C106 C 1.0794(4) 1.0602(5) 0.0778(2) 0.032(2) Uani 1 1 d . . . C107 C 0.3237(3) 0.5765(4) 0.1653(2) 0.0255(18) Uani 1 1 d . . . C108 C 0.4630(4) 1.0551(5) 0.1153(2) 0.033(2) Uani 1 1 d . . . H10E H 0.4425 1.0677 0.1376 0.039 Uiso 1 1 calc R . . C109 C 0.3462(4) 0.7987(4) 0.0887(3) 0.0311(19) Uani 1 1 d . . . C110 C 0.6050(4) 0.4870(4) 0.1165(3) 0.034(2) Uani 1 1 d . . . C111 C 0.9751(4) 0.4549(4) 0.1074(3) 0.0306(19) Uani 1 1 d . . . C112 C 0.5659(4) 0.8753(4) 0.1870(2) 0.0288(18) Uani 1 1 d . . . C113 C 0.6447(4) 0.6204(5) 0.2492(2) 0.031(2) Uani 1 1 d . . . C114 C 0.9215(4) 0.6374(5) 0.0488(3) 0.036(2) Uani 1 1 d . . . H11A H 0.9384 0.6519 0.0253 0.043 Uiso 1 1 calc R . . C115 C 1.0558(4) 0.5714(4) 0.1115(3) 0.0286(18) Uani 1 1 d . . . C116 C 0.4602(4) 0.8536(5) 0.0756(2) 0.034(2) Uani 1 1 d . . . C117 C 0.4306(4) 0.8055(5) 0.0485(3) 0.0331(19) Uani 1 1 d . . . H11B H 0.4485 0.7907 0.0254 0.040 Uiso 1 1 calc R . . C118 C 0.5051(4) 0.4742(4) 0.0767(2) 0.0247(17) Uani 1 1 d . . . C119 C 0.5832(4) 0.3837(4) 0.0766(2) 0.0292(18) Uani 1 1 d . . . C120 C 0.5029(4) 0.6660(5) 0.2982(3) 0.038(2) Uani 1 1 d . . . H12A H 0.4956 0.6169 0.3045 0.057 Uiso 1 1 calc R . . H12B H 0.4682 0.6837 0.2792 0.057 Uiso 1 1 calc R . . H12C H 0.5071 0.6935 0.3234 0.057 Uiso 1 1 calc R . . C121 C 0.5616(4) 0.3497(4) 0.1100(3) 0.0301(19) Uani 1 1 d . . . C122 C 1.0308(3) 0.5512(4) 0.1459(2) 0.0242(17) Uani 1 1 d . . . C123 C 1.0812(4) 0.7026(4) 0.2662(2) 0.0295(19) Uani 1 1 d . . . C124 C 0.8655(4) 0.6647(4) 0.0567(2) 0.0308(19) Uani 1 1 d . . . H12D H 0.8450 0.6986 0.0388 0.037 Uiso 1 1 calc R . . C125 C 0.9680(4) 0.5159(4) 0.1364(2) 0.0281(18) Uani 1 1 d . . . H12E H 0.9508 0.5012 0.1615 0.034 Uiso 1 1 calc R . . C126 C 0.6214(4) 0.8392(4) 0.1921(2) 0.0294(18) Uani 1 1 d . . . C127 C 0.5619(4) 0.8700(4) 0.1136(2) 0.0298(19) Uani 1 1 d . . . C128 C 0.5723(4) 0.4609(4) 0.0751(2) 0.0278(18) Uani 1 1 d . . . H12F H 0.5876 0.4839 0.0514 0.033 Uiso 1 1 calc R . . C129 C 1.0349(3) 1.0396(4) 0.1401(2) 0.0258(17) Uani 1 1 d . . . H12G H 1.0210 1.0622 0.1645 0.031 Uiso 1 1 calc R . . C130 C 0.5220(4) 0.8893(5) 0.0739(3) 0.034(2) Uani 1 1 d . . . H13A H 0.5409 0.8758 0.0493 0.041 Uiso 1 1 calc R . . C131 C 0.9651(4) 0.9247(5) 0.0542(3) 0.035(2) Uani 1 1 d . . . H13B H 0.9789 0.9031 0.0313 0.042 Uiso 1 1 calc R . . C132 C 0.9670(4) 0.3375(5) 0.0824(3) 0.036(2) Uani 1 1 d . . . H13C H 0.9539 0.2906 0.0851 0.043 Uiso 1 1 calc R . . C134 C 1.0622(4) 0.5656(4) 0.1841(2) 0.0269(18) Uani 1 1 d . . . C135 C 1.0603(4) 1.0909(5) 0.1120(2) 0.032(2) Uani 1 1 d . . . C136 C 0.3776(4) 0.3485(5) 0.1402(3) 0.045(2) Uani 1 1 d . . . H13D H 0.3632 0.3286 0.1645 0.067 Uiso 1 1 calc R . . H13E H 0.4100 0.3189 0.1320 0.067 Uiso 1 1 calc R . . H13F H 0.3433 0.3510 0.1179 0.067 Uiso 1 1 calc R . . C137 C 0.4724(3) 0.9254(4) 0.1380(2) 0.0255(17) Uani 1 1 d . . . H13G H 0.4534 0.9389 0.1625 0.031 Uiso 1 1 calc R . . C138 C 1.0039(4) 0.9660(4) 0.0800(3) 0.036(2) Uani 1 1 d . . . C139 C 0.6180(4) 0.2715(4) 0.0562(3) 0.036(2) Uani 1 1 d . . . H13H H 0.6379 0.2440 0.0381 0.043 Uiso 1 1 calc R . . C140 C 1.0727(4) 0.9806(5) 0.0768(2) 0.0315(19) Uani 1 1 d . . . H14A H 1.0870 0.9585 0.0524 0.038 Uiso 1 1 calc R . . C141 C 0.4756(5) 1.1054(5) 0.0863(3) 0.046(2) Uani 1 1 d . . . H14B H 0.4629 1.1524 0.0889 0.055 Uiso 1 1 calc R . . C142 C 0.3170(4) 0.5066(4) 0.0985(3) 0.0290(18) Uani 1 1 d . . . H14C H 0.2892 0.5100 0.0723 0.035 Uiso 1 1 calc R . . H14D H 0.3030 0.4667 0.1139 0.035 Uiso 1 1 calc R . . C143 C 1.0137(4) 0.5547(4) 0.0718(2) 0.0290(19) Uani 1 1 d . . . H14E H 1.0313 0.5698 0.0470 0.035 Uiso 1 1 calc R . . C144 C 1.0656(4) 1.1628(5) 0.1177(3) 0.037(2) Uani 1 1 d . . . H14F H 1.0526 1.1848 0.1406 0.044 Uiso 1 1 calc R . . C145 C 1.1748(3) 0.8819(5) 0.1615(3) 0.0320(19) Uani 1 1 d . . . H14G H 1.2041 0.8452 0.1649 0.038 Uiso 1 1 calc R . . C146 C 1.0911(4) 1.2017(5) 0.0880(3) 0.044(2) Uani 1 1 d . . . H14H H 1.0957 1.2509 0.0912 0.053 Uiso 1 1 calc R . . C147 C 1.0111(4) 0.4261(5) 0.0442(3) 0.038(2) Uani 1 1 d . . . H14I H 1.0289 0.4389 0.0207 0.046 Uiso 1 1 calc R . . C148 C 0.9946(4) 0.3558(5) 0.0497(3) 0.039(2) Uani 1 1 d . . . H14J H 1.0028 0.3213 0.0305 0.047 Uiso 1 1 calc R . . C149 C 0.9049(4) 0.9147(4) 0.0619(2) 0.0303(19) Uani 1 1 d . . . H14K H 0.8783 0.8849 0.0446 0.036 Uiso 1 1 calc R . . C150 C 0.6728(4) 0.5608(5) 0.1616(3) 0.036(2) Uani 1 1 d . . . H15A H 0.7028 0.5968 0.1656 0.043 Uiso 1 1 calc R . . C151 C 0.3740(4) 0.7790(5) 0.0555(3) 0.036(2) Uani 1 1 d . . . H15B H 0.3537 0.7461 0.0368 0.043 Uiso 1 1 calc R . . C152 C 0.8053(3) 0.7421(5) 0.1691(3) 0.033(2) Uani 1 1 d . . . C153 C 0.5337(4) 0.4022(4) 0.1374(2) 0.0300(18) Uani 1 1 d . . . H15C H 0.5182 0.3798 0.1612 0.036 Uiso 1 1 calc R . . C154 C 0.8773(4) 1.0925(5) 0.1426(3) 0.041(2) Uani 1 1 d . . . H15D H 0.8632 1.1137 0.1666 0.061 Uiso 1 1 calc R . . H15E H 0.8425 1.0878 0.1208 0.061 Uiso 1 1 calc R . . H15F H 0.9088 1.1222 0.1333 0.061 Uiso 1 1 calc R . . C155 C 1.1429(4) 0.6206(5) 0.1542(3) 0.035(2) Uani 1 1 d . . . H15G H 1.1813 0.6441 0.1570 0.042 Uiso 1 1 calc R . . C157 C 0.5235(4) 1.0186(4) 0.0492(2) 0.0302(19) Uani 1 1 d . . . H15H H 0.5448 1.0062 0.0272 0.036 Uiso 1 1 calc R . . C159 C 0.5973(5) 0.2400(5) 0.0890(3) 0.044(2) Uani 1 1 d . . . H15I H 0.6022 0.1911 0.0930 0.053 Uiso 1 1 calc R . . C161 C 1.1042(4) 1.0987(5) 0.0494(3) 0.042(2) Uani 1 1 d . . . H16A H 1.1176 1.0767 0.0265 0.050 Uiso 1 1 calc R . . C162 C 0.4042(4) 0.5245(5) 0.0569(3) 0.036(2) Uani 1 1 d . . . H16B H 0.3778 0.5532 0.0387 0.044 Uiso 1 1 calc R . . C163 C 0.5575(4) 0.9628(5) 0.2370(3) 0.036(2) Uani 1 1 d . . . H16C H 0.5367 0.9732 0.2606 0.054 Uiso 1 1 calc R . . H16D H 0.5468 0.9985 0.2159 0.054 Uiso 1 1 calc R . . H16E H 0.6020 0.9628 0.2454 0.054 Uiso 1 1 calc R . . C164 C 0.8188(4) 0.5043(5) 0.1481(3) 0.041(2) Uani 1 1 d . . . H16F H 0.8034 0.4920 0.1736 0.061 Uiso 1 1 calc R . . H16G H 0.8489 0.4693 0.1422 0.061 Uiso 1 1 calc R . . H16H H 0.7845 0.5054 0.1258 0.061 Uiso 1 1 calc R . . C165 C 1.1096(4) 1.1700(5) 0.0545(3) 0.046(3) Uani 1 1 d . . . H16I H 1.1261 1.1975 0.0347 0.055 Uiso 1 1 calc R . . C166 C 0.5061(5) 1.0871(5) 0.0544(3) 0.049(3) Uani 1 1 d . . . H16J H 0.5154 1.1218 0.0357 0.058 Uiso 1 1 calc R . . C167 C 1.1160(5) 1.0621(4) 0.2366(3) 0.046(2) Uani 1 1 d . . . H16K H 1.0990 1.0787 0.2607 0.069 Uiso 1 1 calc R . . H16L H 1.1054 1.0950 0.2141 0.069 Uiso 1 1 calc R . . H16M H 1.1608 1.0587 0.2430 0.069 Uiso 1 1 calc R . . C4A C 0.3421(4) 0.5228(5) 0.3556(3) 0.045(2) Uani 1 1 d . . . H4AA H 0.3677 0.4796 0.3605 0.054 Uiso 1 1 calc R . . C2A C 0.1538(5) 0.4197(6) 0.1401(4) 0.057(3) Uani 1 1 d . . . H2AA H 0.1278 0.4627 0.1354 0.068 Uiso 1 1 calc R . . C172 C 0.6103(4) 0.3427(5) 0.0490(2) 0.033(2) Uani 1 1 d . . . H17A H 0.6234 0.3633 0.0255 0.040 Uiso 1 1 calc R . . C173 C 0.6474(4) 0.8212(4) 0.1577(3) 0.033(2) Uani 1 1 d . . . H17B H 0.6859 0.7980 0.1609 0.040 Uiso 1 1 calc R . . C6A C 0.2229(5) 0.7745(6) 0.3442(3) 0.056(3) Uani 1 1 d . . . H6AA H 0.1901 0.7809 0.3203 0.067 Uiso 1 1 calc R . . C175 C 0.6115(4) 0.3794(5) 0.2353(3) 0.040(2) Uani 1 1 d . . . H17C H 0.5935 0.3630 0.2590 0.060 Uiso 1 1 calc R . . H17D H 0.6562 0.3827 0.2424 0.060 Uiso 1 1 calc R . . H17E H 0.6016 0.3464 0.2127 0.060 Uiso 1 1 calc R . . C176 C 1.0534(4) 0.4783(5) 0.2340(3) 0.040(2) Uani 1 1 d . . . H17F H 1.0339 0.4685 0.2583 0.060 Uiso 1 1 calc R . . H17G H 1.0981 0.4761 0.2412 0.060 Uiso 1 1 calc R . . H17H H 1.0401 0.4434 0.2129 0.060 Uiso 1 1 calc R . . C1A C 0.7211(5) 0.8336(6) -0.1557(3) 0.055(3) Uani 1 1 d . . . H1AA H 0.6903 0.8388 -0.1808 0.066 Uiso 1 1 calc R . . C180 C 0.3212(4) 0.9377(5) 0.1442(3) 0.038(2) Uani 1 1 d . . . H18A H 0.3031 0.9497 0.1688 0.057 Uiso 1 1 calc R . . H18B H 0.2889 0.9366 0.1206 0.057 Uiso 1 1 calc R . . H18C H 0.3519 0.9730 0.1398 0.057 Uiso 1 1 calc R . . C3A C 0.4870(15) 0.6692(7) 0.1627(7) 0.217(16) Uani 1 1 d . . . H3A H 0.4451 0.6629 0.1469 0.260 Uiso 1 1 calc R . . C7A C 0.6752(7) 0.9603(9) -0.0271(4) 0.091(5) Uani 1 1 d . . . H7AA H 0.6482 0.9435 -0.0520 0.110 Uiso 1 1 calc R . . C5A C 0.0178(15) 0.2732(9) 0.3376(6) 0.204(15) Uani 1 1 d . . . H5A H 0.0596 0.2814 0.3531 0.245 Uiso 1 1 calc R . . Cl24 Cl 0.0993(2) 0.7250(3) 0.53367(12) 0.1102(15) Uani 1 1 d . . . Cl23 Cl 0.06716(19) 0.6403(3) 0.46269(12) 0.1082(15) Uani 1 1 d . . . Cl27 Cl 0.5922(3) 0.6513(3) 0.03284(15) 0.154(2) Uani 1 1 d . . . Cl22 Cl 0.1932(2) 0.6541(4) 0.49809(16) 0.148(2) Uani 1 1 d . . . Cl26 Cl 0.5700(3) 0.7322(3) -0.03751(15) 0.161(3) Uani 1 1 d . . . Cl25 Cl 0.6834(3) 0.6660(6) -0.0174(2) 0.254(6) Uani 1 1 d . . . Cl30 Cl 0.2037(6) 0.8566(5) 0.4866(4) 0.338(8) Uani 1 1 d . . . C8A C 0.1222(6) 0.6944(9) 0.4884(5) 0.093(5) Uani 1 1 d . . . H8AA H 0.1265 0.7358 0.4706 0.112 Uiso 1 1 calc R . . C9A C 0.6078(7) 0.6622(7) -0.0159(4) 0.075(4) Uani 1 1 d . . . H9AA H 0.5917 0.6201 -0.0319 0.090 Uiso 1 1 calc R . . Cl29 Cl 0.1581(2) 0.9745(4) 0.51398(16) 0.146(2) Uani 1 1 d . . . Cl28 Cl 0.2535(3) 0.9914(6) 0.4679(2) 0.262(6) Uani 1 1 d . . . C10A C 0.1922(7) 0.9298(18) 0.4643(7) 0.28(2) Uani 1 1 d . . . H10F H 0.1636 0.9295 0.4380 0.340 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl15 0.0409(13) 0.0391(13) 0.0599(15) -0.0029(12) -0.0007(11) -0.0003(10) Cl9 0.0392(12) 0.0411(14) 0.0586(15) -0.0004(12) 0.0020(11) -0.0013(10) Cl12 0.0404(13) 0.0578(16) 0.0532(15) 0.0002(12) 0.0148(11) -0.0126(11) Cl6 0.0406(13) 0.0554(16) 0.0594(16) -0.0006(13) 0.0163(12) -0.0113(11) Cl8 0.0455(14) 0.0411(14) 0.0667(17) 0.0015(12) -0.0034(12) -0.0025(11) Cl14 0.0493(14) 0.0384(14) 0.0678(17) 0.0043(12) -0.0033(12) -0.0002(11) Cl11 0.0475(15) 0.073(2) 0.0702(18) -0.0108(15) 0.0089(13) -0.0191(14) Cl5 0.0435(14) 0.0657(19) 0.078(2) -0.0115(15) 0.0064(13) -0.0136(13) Cl3 0.0687(19) 0.0500(17) 0.097(2) 0.0080(16) 0.0160(17) -0.0012(14) Cl18 0.0677(19) 0.0583(19) 0.108(3) 0.0091(18) 0.0134(18) 0.0055(15) Cl10 0.0577(17) 0.124(3) 0.0515(17) 0.0122(18) 0.0131(14) -0.0299(18) Cl2 0.0612(19) 0.059(2) 0.128(3) -0.020(2) -0.0113(19) 0.0219(15) Cl4 0.0619(19) 0.130(3) 0.0545(17) 0.0131(19) 0.0167(15) -0.0245(19) Cl7 0.120(3) 0.096(3) 0.077(2) 0.018(2) 0.051(2) 0.016(2) Cl13 0.125(3) 0.091(3) 0.085(3) 0.004(2) 0.057(2) -0.003(2) Cl17 0.070(2) 0.075(2) 0.152(4) -0.029(2) -0.025(2) 0.0215(19) O1 0.024(3) 0.043(4) 0.028(3) -0.003(3) 0.001(2) 0.008(3) O2 0.027(3) 0.030(3) 0.032(3) -0.009(3) 0.006(2) 0.005(2) O3 0.032(3) 0.039(4) 0.036(3) -0.003(3) 0.020(3) -0.004(3) O4 0.035(3) 0.033(3) 0.028(3) -0.002(3) 0.008(2) 0.002(3) O5 0.043(3) 0.026(3) 0.029(3) 0.001(2) 0.009(3) -0.001(3) O6 0.031(3) 0.031(3) 0.031(3) -0.001(3) 0.012(2) 0.002(2) O7 0.038(3) 0.036(3) 0.031(3) -0.008(3) 0.003(3) 0.001(3) O8 0.035(3) 0.039(4) 0.034(3) 0.001(3) 0.011(3) -0.001(3) O9 0.030(3) 0.027(3) 0.036(3) -0.004(3) 0.013(2) -0.003(2) O10 0.031(3) 0.034(3) 0.026(3) -0.007(2) 0.010(2) -0.004(2) O11 0.026(3) 0.037(3) 0.030(3) 0.002(3) 0.003(2) -0.008(2) O12 0.037(3) 0.024(3) 0.029(3) 0.004(2) 0.006(2) 0.002(2) O13 0.042(3) 0.029(3) 0.040(3) -0.002(3) 0.011(3) -0.010(3) O14 0.029(3) 0.042(4) 0.028(3) 0.009(3) 0.010(2) 0.004(3) O15 0.037(3) 0.036(3) 0.030(3) 0.000(3) 0.001(3) -0.002(3) O16 0.043(3) 0.034(3) 0.029(3) 0.004(3) 0.011(3) 0.002(3) Cl1 0.121(3) 0.112(3) 0.092(3) -0.034(2) 0.053(2) -0.050(3) Cl21 0.090(3) 0.078(3) 0.128(3) 0.024(2) 0.010(2) -0.002(2) Cl16 0.175(5) 0.185(5) 0.095(3) -0.026(3) 0.073(3) -0.072(4) Cl20 0.079(2) 0.105(3) 0.115(3) 0.047(3) 0.030(2) 0.030(2) Cl19 0.067(2) 0.207(6) 0.138(4) -0.029(4) 0.043(3) 0.016(3) C40 0.024(4) 0.033(5) 0.029(4) -0.003(4) 0.010(3) -0.007(3) C42 0.026(4) 0.017(4) 0.034(4) 0.004(3) 0.004(3) -0.020(3) C44 0.028(4) 0.039(5) 0.027(4) -0.002(4) -0.007(3) 0.001(4) C46 0.021(4) 0.030(5) 0.030(4) -0.002(4) 0.007(3) 0.003(3) C47 0.029(4) 0.018(4) 0.031(4) -0.008(3) 0.009(3) -0.003(3) C48 0.026(4) 0.015(4) 0.038(5) 0.002(3) 0.003(3) 0.006(3) C49 0.025(4) 0.044(5) 0.035(5) -0.005(4) 0.003(4) 0.000(4) C50 0.020(4) 0.041(5) 0.024(4) 0.007(4) 0.001(3) -0.009(3) C51 0.025(4) 0.039(5) 0.014(4) -0.006(3) -0.001(3) 0.010(3) C52 0.019(4) 0.055(6) 0.025(4) 0.007(4) 0.007(3) -0.022(4) C53 0.011(3) 0.046(5) 0.025(4) 0.003(4) 0.010(3) -0.002(3) C54 0.031(4) 0.016(4) 0.032(4) -0.011(3) -0.011(3) 0.027(3) C55 0.019(4) 0.055(6) 0.024(4) -0.003(4) 0.008(3) 0.001(4) C56 0.030(4) 0.035(5) 0.026(4) 0.004(4) 0.005(3) -0.004(4) C57 0.042(5) 0.024(4) 0.029(4) 0.001(4) 0.026(4) 0.004(4) C59 0.014(4) 0.043(5) 0.029(4) 0.003(4) 0.000(3) -0.005(3) C60 0.030(4) 0.023(4) 0.046(5) -0.002(4) 0.012(4) -0.008(3) C61 0.016(4) 0.024(4) 0.035(4) -0.010(4) -0.006(3) 0.004(3) C62 0.020(4) 0.033(5) 0.040(5) -0.004(4) 0.011(4) 0.002(3) C63 0.021(4) 0.041(5) 0.036(5) -0.003(4) 0.011(3) 0.005(4) C64 0.013(4) 0.050(5) 0.024(4) -0.010(4) 0.006(3) 0.002(3) C65 0.029(4) 0.040(5) 0.024(4) -0.010(4) 0.001(3) 0.020(4) C66 0.030(4) 0.035(5) 0.024(4) 0.007(4) 0.005(3) 0.002(4) C67 0.022(4) 0.022(4) 0.036(5) 0.004(4) 0.003(3) -0.003(3) C68 0.028(4) 0.023(4) 0.035(5) 0.010(4) 0.002(4) -0.004(3) C69 0.027(4) 0.030(5) 0.032(4) 0.000(4) 0.002(3) 0.005(3) C70 0.023(4) 0.040(5) 0.032(4) -0.006(4) 0.012(3) -0.001(4) C72 0.028(4) 0.007(3) 0.030(4) 0.001(3) -0.001(3) -0.022(3) C73 0.024(4) 0.041(5) 0.028(4) 0.005(4) 0.001(3) 0.004(4) C74 0.022(4) 0.044(5) 0.040(5) -0.004(4) 0.014(4) -0.008(4) C75 0.031(4) 0.040(5) 0.016(4) 0.001(4) 0.001(3) -0.010(4) C76 0.022(4) 0.022(4) 0.036(5) 0.001(4) 0.008(3) 0.006(3) C77 0.021(4) 0.031(5) 0.041(5) -0.003(4) 0.013(4) 0.013(3) C78 0.026(4) 0.026(4) 0.033(4) -0.010(4) -0.001(3) -0.005(3) C79 0.031(4) 0.028(5) 0.030(4) 0.005(4) 0.007(4) 0.002(3) C80 0.022(4) 0.033(5) 0.033(4) 0.004(4) 0.006(3) 0.000(3) C81 0.030(4) 0.020(4) 0.020(4) -0.006(3) 0.012(3) 0.002(3) C82 0.026(4) 0.058(6) 0.026(4) -0.004(4) -0.003(3) -0.005(4) C83 0.023(4) 0.046(6) 0.033(5) 0.001(4) 0.010(4) 0.010(4) C84 0.034(5) 0.050(6) 0.025(4) 0.010(4) 0.007(4) 0.008(4) C85 0.018(4) 0.046(5) 0.029(4) -0.002(4) 0.004(3) 0.007(4) C86 0.012(4) 0.042(5) 0.037(5) 0.003(4) 0.004(3) 0.003(3) C87 0.044(5) 0.044(6) 0.025(4) -0.005(4) 0.011(4) -0.009(4) C88 0.027(4) 0.022(4) 0.038(5) 0.007(4) 0.007(4) -0.007(3) C89 0.033(5) 0.054(6) 0.024(4) -0.011(4) -0.001(4) 0.006(4) C90 0.027(4) 0.025(4) 0.035(5) -0.003(4) 0.006(4) 0.003(3) C91 0.027(4) 0.033(5) 0.035(5) 0.006(4) 0.001(4) -0.010(4) C92 0.020(4) 0.041(5) 0.027(4) -0.008(4) 0.008(3) 0.001(3) C93 0.035(4) 0.017(4) 0.033(4) -0.003(3) 0.002(4) -0.001(3) C94 0.043(5) 0.031(5) 0.039(5) 0.005(4) 0.013(4) 0.004(4) C95 0.026(4) 0.019(4) 0.034(4) -0.003(3) 0.009(3) 0.003(3) C96 0.037(5) 0.033(5) 0.028(4) 0.005(4) 0.011(4) 0.001(4) C97 0.023(4) 0.036(5) 0.030(4) 0.001(4) -0.004(3) -0.002(3) C98 0.030(4) 0.031(5) 0.018(4) -0.002(3) 0.001(3) 0.004(3) C99 0.026(4) 0.025(4) 0.030(4) 0.000(4) 0.002(3) -0.004(3) C100 0.033(4) 0.024(4) 0.021(4) 0.003(3) 0.001(3) 0.008(3) C101 0.038(5) 0.029(5) 0.046(5) 0.005(4) 0.010(4) -0.007(4) C102 0.032(4) 0.016(4) 0.038(5) -0.001(4) 0.004(4) 0.003(3) C103 0.026(4) 0.057(6) 0.019(4) 0.002(4) 0.002(3) 0.006(4) C104 0.042(5) 0.032(5) 0.032(5) -0.005(4) 0.006(4) -0.016(4) C105 0.027(4) 0.015(4) 0.034(4) 0.009(3) -0.003(3) -0.001(3) C106 0.022(4) 0.046(5) 0.026(4) 0.008(4) -0.004(3) -0.001(4) C107 0.017(4) 0.019(4) 0.038(5) 0.013(4) -0.004(3) -0.005(3) C108 0.032(4) 0.040(5) 0.024(4) 0.003(4) -0.005(3) -0.002(4) C109 0.024(4) 0.033(5) 0.036(5) 0.011(4) 0.006(4) -0.002(3) C110 0.027(4) 0.027(5) 0.052(6) -0.006(4) 0.018(4) 0.002(3) C111 0.022(4) 0.035(5) 0.033(5) -0.003(4) -0.004(3) 0.008(3) C112 0.030(4) 0.033(5) 0.024(4) -0.002(4) 0.002(3) -0.007(4) C113 0.023(4) 0.049(6) 0.021(4) -0.015(4) 0.004(3) -0.011(4) C114 0.049(5) 0.034(5) 0.029(5) 0.003(4) 0.018(4) 0.001(4) C115 0.025(4) 0.027(4) 0.035(5) 0.001(4) 0.009(3) 0.003(3) C116 0.023(4) 0.055(6) 0.026(4) 0.006(4) 0.011(3) -0.002(4) C117 0.035(5) 0.036(5) 0.028(4) -0.004(4) 0.001(4) -0.001(4) C118 0.032(4) 0.021(4) 0.020(4) 0.006(3) 0.002(3) -0.004(3) C119 0.034(4) 0.029(5) 0.027(4) 0.009(4) 0.015(4) -0.004(4) C120 0.042(5) 0.038(5) 0.037(5) 0.005(4) 0.019(4) 0.004(4) C121 0.030(4) 0.023(4) 0.036(5) 0.001(4) -0.003(4) -0.007(3) C122 0.022(4) 0.030(4) 0.020(4) -0.006(3) 0.001(3) -0.002(3) C123 0.037(5) 0.020(4) 0.028(4) -0.002(3) -0.007(4) 0.005(3) C124 0.036(5) 0.027(5) 0.028(4) 0.002(4) 0.002(4) 0.012(4) C125 0.032(4) 0.034(5) 0.020(4) 0.001(4) 0.012(3) 0.004(4) C126 0.028(4) 0.030(5) 0.030(4) -0.002(4) 0.001(3) 0.001(3) C127 0.024(4) 0.034(5) 0.032(4) 0.014(4) 0.005(3) 0.000(3) C128 0.030(4) 0.029(5) 0.025(4) -0.001(3) 0.004(3) -0.007(3) C129 0.024(4) 0.022(4) 0.031(4) 0.002(3) 0.006(3) 0.007(3) C130 0.021(4) 0.053(6) 0.031(5) -0.007(4) 0.015(3) 0.001(4) C131 0.039(5) 0.037(5) 0.031(5) -0.008(4) 0.011(4) 0.005(4) C132 0.035(5) 0.038(5) 0.036(5) -0.001(4) 0.006(4) -0.002(4) C134 0.027(4) 0.021(4) 0.036(5) -0.004(4) 0.016(4) -0.002(3) C135 0.034(5) 0.045(6) 0.017(4) -0.005(4) 0.002(3) -0.004(4) C136 0.042(5) 0.054(6) 0.038(5) 0.011(5) 0.003(4) -0.008(5) C137 0.018(4) 0.035(5) 0.024(4) -0.003(3) 0.003(3) 0.003(3) C138 0.036(5) 0.027(5) 0.042(5) 0.008(4) 0.000(4) 0.005(4) C139 0.056(6) 0.018(4) 0.034(5) -0.007(4) 0.007(4) 0.012(4) C140 0.029(4) 0.044(5) 0.024(4) -0.005(4) 0.010(3) 0.007(4) C141 0.056(6) 0.034(5) 0.042(6) 0.004(4) -0.010(5) -0.013(5) C142 0.026(4) 0.027(4) 0.034(5) 0.007(4) 0.004(3) -0.003(3) C143 0.041(5) 0.014(4) 0.029(4) -0.007(3) -0.004(4) 0.002(3) C144 0.028(4) 0.039(5) 0.042(5) -0.006(4) 0.003(4) -0.002(4) C145 0.019(4) 0.039(5) 0.039(5) 0.001(4) 0.005(3) 0.007(3) C146 0.052(6) 0.030(5) 0.048(6) -0.008(4) 0.001(5) 0.009(4) C147 0.034(5) 0.049(6) 0.032(5) -0.002(4) 0.006(4) 0.017(4) C148 0.048(5) 0.046(6) 0.024(4) -0.010(4) 0.007(4) 0.009(4) C149 0.029(4) 0.034(5) 0.028(4) 0.005(4) 0.004(3) -0.006(4) C150 0.031(5) 0.042(5) 0.035(5) -0.003(4) 0.004(4) -0.005(4) C151 0.038(5) 0.035(5) 0.035(5) 0.000(4) 0.002(4) -0.001(4) C152 0.014(4) 0.055(6) 0.030(4) 0.008(4) 0.006(3) 0.011(4) C153 0.030(4) 0.034(5) 0.027(4) 0.007(4) 0.010(3) 0.000(4) C154 0.040(5) 0.039(5) 0.042(5) -0.001(4) 0.002(4) 0.016(4) C155 0.028(4) 0.041(5) 0.035(5) 0.012(4) 0.003(4) 0.001(4) C157 0.028(4) 0.034(5) 0.028(4) 0.005(4) 0.002(3) -0.002(4) C159 0.056(6) 0.032(5) 0.044(6) -0.006(4) 0.007(5) 0.009(4) C161 0.044(5) 0.043(6) 0.039(5) -0.001(4) 0.009(4) 0.003(4) C162 0.046(5) 0.032(5) 0.029(5) -0.001(4) -0.002(4) -0.006(4) C163 0.041(5) 0.034(5) 0.034(5) -0.012(4) 0.008(4) -0.005(4) C164 0.033(5) 0.043(6) 0.047(6) -0.001(4) 0.005(4) -0.005(4) C165 0.039(5) 0.053(7) 0.048(6) 0.025(5) 0.008(4) -0.006(4) C166 0.059(6) 0.049(6) 0.034(5) 0.013(5) -0.005(5) -0.020(5) C167 0.054(6) 0.021(5) 0.060(6) -0.019(4) -0.002(5) -0.002(4) C4A 0.032(5) 0.042(6) 0.061(6) 0.009(5) 0.003(4) -0.005(4) C2A 0.038(5) 0.056(7) 0.077(8) 0.015(6) 0.011(5) 0.003(5) C172 0.038(5) 0.044(5) 0.019(4) -0.007(4) 0.011(4) 0.004(4) C173 0.023(4) 0.031(5) 0.049(5) 0.007(4) 0.014(4) 0.002(3) C6A 0.041(6) 0.065(7) 0.058(7) 0.001(6) -0.009(5) 0.005(5) C175 0.038(5) 0.055(6) 0.030(5) 0.012(4) 0.011(4) 0.004(4) C176 0.047(5) 0.028(5) 0.043(5) 0.002(4) 0.003(4) 0.000(4) C1A 0.064(7) 0.046(6) 0.056(7) 0.016(5) 0.010(5) 0.005(5) C180 0.037(5) 0.032(5) 0.049(6) -0.002(4) 0.019(4) 0.001(4) C3A 0.50(5) 0.018(7) 0.19(2) 0.026(9) 0.27(3) 0.042(14) C7A 0.090(10) 0.124(14) 0.060(8) -0.015(9) 0.008(7) -0.010(10) C5A 0.46(4) 0.074(12) 0.128(16) 0.045(11) 0.22(2) 0.066(18) Cl24 0.141(4) 0.122(4) 0.067(2) 0.009(2) 0.014(2) 0.033(3) Cl23 0.084(3) 0.160(4) 0.077(2) -0.004(3) 0.000(2) -0.040(3) Cl27 0.252(7) 0.134(4) 0.082(3) 0.040(3) 0.044(4) -0.033(4) Cl22 0.079(3) 0.231(7) 0.123(4) -0.057(4) -0.022(3) 0.031(3) Cl26 0.269(8) 0.113(4) 0.090(3) 0.034(3) -0.009(4) 0.074(4) Cl25 0.085(4) 0.505(16) 0.163(6) -0.163(8) -0.018(4) 0.033(6) Cl30 0.379(16) 0.187(9) 0.383(16) -0.116(10) -0.167(13) -0.028(9) C8A 0.069(9) 0.123(13) 0.087(10) 0.018(10) 0.008(8) 0.006(9) C9A 0.097(10) 0.068(9) 0.059(8) 0.000(6) 0.006(7) -0.017(7) Cl29 0.083(3) 0.247(7) 0.111(4) -0.041(4) 0.026(3) 0.029(4) Cl28 0.089(4) 0.512(16) 0.188(6) 0.231(9) 0.026(4) 0.012(6) C10A 0.078(11) 0.53(5) 0.21(2) 0.33(3) -0.113(13) -0.144(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl15 C5A 1.677(16) . ? Cl9 C3A 1.680(13) . ? Cl12 C4A 1.735(9) . ? Cl6 C2A 1.745(11) . ? Cl8 C3A 1.716(13) . ? Cl14 C5A 1.696(15) . ? Cl11 C4A 1.778(10) . ? Cl5 C2A 1.757(11) . ? Cl3 C1A 1.754(11) . ? Cl18 C6A 1.784(12) . ? Cl10 C4A 1.746(11) . ? Cl2 C1A 1.731(11) . ? Cl4 C2A 1.741(12) . ? Cl7 C3A 1.620(14) . ? Cl13 C5A 1.647(14) . ? Cl17 C6A 1.704(11) . ? O1 C47 1.413(9) . ? O1 C167 1.448(10) . ? O2 C44 1.400(10) . ? O2 C154 1.464(10) . ? O3 C70 1.398(10) . ? O3 C164 1.437(10) . ? O4 C134 1.405(9) . ? O4 C176 1.438(10) . ? O5 C123 1.385(10) . ? O5 H5 0.8401 . ? O6 C81 1.373(9) . ? O6 H6 0.8400 . ? O7 C55 1.378(10) . ? O7 H7 0.8400 . ? O8 C152 1.387(10) . ? O8 H8 0.8400 . ? O9 C100 1.405(9) . ? O9 C180 1.436(10) . ? O10 C112 1.393(9) . ? O10 C163 1.450(10) . ? O11 C60 1.400(10) . ? O11 C136 1.452(11) . ? O12 C46 1.400(10) . ? O12 C175 1.437(10) . ? O13 C82 1.408(11) . ? O13 H13 0.8401 . ? O14 C64 1.364(10) . ? O14 H14 0.8399 . ? O15 C107 1.373(9) . ? O15 H15 0.8400 . ? O16 C76 1.383(10) . ? O16 H16 0.8400 . ? Cl1 C1A 1.743(11) . ? Cl21 C7A 1.758(16) . ? Cl16 C6A 1.694(12) . ? Cl20 C7A 1.692(17) . ? Cl19 C7A 1.769(16) . ? C40 C152 1.408(12) . ? C40 C55 1.408(12) . ? C40 C89 1.499(11) . ? C42 C65 1.376(11) . ? C42 C72 1.408(11) . ? C42 H42A 0.9500 . ? C44 C51 1.379(11) . ? C44 C84 1.401(12) . ? C46 C79 1.392(11) . ? C46 C95 1.395(11) . ? C47 C69 1.399(11) . ? C47 C68 1.407(11) . ? C48 C126 1.529(11) . ? C48 C54 1.528(11) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C127 1.388(11) . ? C49 C173 1.391(12) . ? C49 H49A 0.9500 . ? C50 C76 1.381(11) . ? C50 C107 1.389(12) . ? C50 C94 1.516(11) . ? C51 C138 1.409(12) . ? C51 C129 1.524(11) . ? C52 C113 1.388(12) . ? C52 C54 1.398(11) . ? C52 H52A 0.9500 . ? C53 C76 1.402(11) . ? C53 C59 1.409(12) . ? C53 C66 1.536(11) . ? C54 C64 1.394(11) . ? C55 C86 1.406(11) . ? C56 C123 1.393(12) . ? C56 C81 1.396(11) . ? C56 C101 1.539(12) . ? C57 C115 1.392(11) . ? C57 C155 1.403(12) . ? C57 H57A 0.9500 . ? C59 C97 1.414(12) . ? C59 H59A 0.9500 . ? C60 C102 1.402(11) . ? C60 C105 1.410(11) . ? C61 C98 1.366(11) . ? C61 C152 1.420(11) . ? C61 C85 1.518(11) . ? C62 C92 1.385(11) . ? C62 C145 1.396(12) . ? C62 H62A 0.9500 . ? C63 C72 1.475(10) . ? C63 C68 1.529(11) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C80 1.435(12) . ? C65 C123 1.419(12) . ? C65 C83 1.546(11) . ? C66 C109 1.520(11) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C157 1.365(11) . ? C67 C78 1.404(11) . ? C67 C130 1.552(12) . ? C68 C145 1.372(12) . ? C69 C92 1.395(11) . ? C69 C129 1.544(10) . ? C70 C75 1.371(11) . ? C70 C99 1.400(12) . ? C72 C81 1.403(11) . ? C73 C84 1.512(11) . ? C73 C86 1.545(12) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C150 1.401(12) . ? C74 C110 1.402(12) . ? C74 H74A 0.9500 . ? C75 C93 1.414(11) . ? C75 C125 1.531(11) . ? C77 C134 1.390(11) . ? C77 C155 1.392(12) . ? C77 C83 1.527(12) . ? C78 C108 1.385(12) . ? C78 C137 1.524(11) . ? C79 C150 1.405(12) . ? C79 C90 1.520(11) . ? C80 C82 1.393(12) . ? C80 C120 1.473(11) . ? C82 C113 1.397(12) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 C149 1.412(12) . ? C85 C99 1.523(11) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 C98 1.388(12) . ? C87 C118 1.379(12) . ? C87 C162 1.414(13) . ? C87 H87A 0.9500 . ? C88 C100 1.368(11) . ? C88 C116 1.409(12) . ? C88 C137 1.531(11) . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 C113 1.552(11) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 C112 1.383(11) . ? C91 C127 1.416(12) . ? C91 C137 1.541(11) . ? C92 C140 1.525(11) . ? C93 C114 1.385(12) . ? C93 C143 1.519(11) . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C95 C110 1.376(12) . ? C95 C153 1.535(11) . ? C96 C111 1.380(12) . ? C96 C132 1.390(12) . ? C96 H96A 0.9500 . ? C97 C107 1.411(11) . ? C97 C142 1.496(12) . ? C98 H98A 0.9500 . ? C99 C124 1.420(11) . ? C100 C109 1.411(12) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C102 C118 1.388(11) . ? C102 C153 1.537(11) . ? C103 C147 1.384(12) . ? C103 C111 1.423(12) . ? C103 C143 1.520(12) . ? C104 C121 1.369(12) . ? C104 C159 1.379(13) . ? C104 H10D 0.9500 . ? C105 C162 1.405(12) . ? C105 C142 1.515(11) . ? C106 C161 1.369(12) . ? C106 C135 1.393(12) . ? C106 C140 1.531(12) . ? C108 C141 1.414(13) . ? C108 H10E 0.9500 . ? C109 C151 1.385(12) . ? C110 C128 1.538(12) . ? C111 C125 1.536(11) . ? C112 C126 1.391(11) . ? C114 C124 1.397(12) . ? C114 H11A 0.9500 . ? C115 C122 1.388(11) . ? C115 C143 1.531(11) . ? C116 C117 1.383(12) . ? C116 C130 1.529(11) . ? C117 C151 1.394(12) . ? C117 H11B 0.9500 . ? C118 C128 1.509(11) . ? C119 C172 1.402(11) . ? C119 C121 1.421(11) . ? C119 C128 1.496(11) . ? C120 H12A 0.9800 . ? C120 H12B 0.9800 . ? C120 H12C 0.9800 . ? C121 C153 1.537(12) . ? C122 C134 1.382(11) . ? C122 C125 1.529(11) . ? C124 H12D 0.9500 . ? C125 H12E 1.0000 . ? C126 C173 1.388(12) . ? C127 C130 1.520(11) . ? C128 H12F 1.0000 . ? C129 C135 1.512(11) . ? C129 H12G 1.0000 . ? C130 H13A 1.0000 . ? C131 C138 1.371(12) . ? C131 C149 1.396(12) . ? C131 H13B 0.9500 . ? C132 C148 1.361(12) . ? C132 H13C 0.9500 . ? C135 C144 1.390(12) . ? C136 H13D 0.9800 . ? C136 H13E 0.9800 . ? C136 H13F 0.9800 . ? C137 H13G 1.0000 . ? C138 C140 1.557(12) . ? C139 C159 1.374(13) . ? C139 C172 1.389(12) . ? C139 H13H 0.9500 . ? C140 H14A 1.0000 . ? C141 C166 1.375(15) . ? C141 H14B 0.9500 . ? C142 H14C 0.9900 . ? C142 H14D 0.9900 . ? C143 H14E 1.0000 . ? C144 C146 1.412(14) . ? C144 H14F 0.9500 . ? C145 H14G 0.9500 . ? C146 C165 1.375(14) . ? C146 H14H 0.9500 . ? C147 C148 1.411(13) . ? C147 H14I 0.9500 . ? C148 H14J 0.9500 . ? C149 H14K 0.9500 . ? C150 H15A 0.9500 . ? C151 H15B 0.9500 . ? C153 H15C 1.0000 . ? C154 H15D 0.9800 . ? C154 H15E 0.9800 . ? C154 H15F 0.9800 . ? C155 H15G 0.9500 . ? C157 C166 1.382(14) . ? C157 H15H 0.9500 . ? C159 H15I 0.9500 . ? C161 C165 1.378(14) . ? C161 H16A 0.9500 . ? C162 H16B 0.9500 . ? C163 H16C 0.9800 . ? C163 H16D 0.9800 . ? C163 H16E 0.9800 . ? C164 H16F 0.9800 . ? C164 H16G 0.9800 . ? C164 H16H 0.9800 . ? C165 H16I 0.9500 . ? C166 H16J 0.9500 . ? C167 H16K 0.9800 . ? C167 H16L 0.9800 . ? C167 H16M 0.9800 . ? C4A H4AA 1.0000 . ? C2A H2AA 1.0000 . ? C172 H17A 0.9500 . ? C173 H17B 0.9500 . ? C6A H6AA 1.0000 . ? C175 H17C 0.9800 . ? C175 H17D 0.9800 . ? C175 H17E 0.9800 . ? C176 H17F 0.9800 . ? C176 H17G 0.9800 . ? C176 H17H 0.9800 . ? C1A H1AA 1.0000 . ? C180 H18A 0.9800 . ? C180 H18B 0.9800 . ? C180 H18C 0.9800 . ? C3A H3A 1.0000 . ? C7A H7AA 1.0000 . ? C5A H5A 1.0000 . ? Cl24 C8A 1.748(16) . ? Cl23 C8A 1.724(16) . ? Cl27 C9A 1.709(13) . ? Cl22 C8A 1.732(15) . ? Cl26 C9A 1.682(14) . ? Cl25 C9A 1.674(15) . ? Cl30 C10A 1.59(2) . ? C8A H8AA 1.0000 . ? C9A H9AA 1.0000 . ? Cl29 C10A 2.08(4) . ? Cl28 C10A 1.78(2) . ? C10A H10F 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C47 O1 C167 113.8(7) . . ? C44 O2 C154 111.3(6) . . ? C70 O3 C164 113.6(7) . . ? C134 O4 C176 113.5(6) . . ? C123 O5 H5 108.1 . . ? C81 O6 H6 112.3 . . ? C55 O7 H7 107.3 . . ? C152 O8 H8 114.6 . . ? C100 O9 C180 113.3(6) . . ? C112 O10 C163 113.5(6) . . ? C60 O11 C136 112.2(6) . . ? C46 O12 C175 114.4(6) . . ? C82 O13 H13 118.8 . . ? C64 O14 H14 102.6 . . ? C107 O15 H15 112.2 . . ? C76 O16 H16 114.5 . . ? C152 C40 C55 116.8(7) . . ? C152 C40 C89 120.6(8) . . ? C55 C40 C89 122.2(8) . . ? C65 C42 C72 123.2(7) . . ? C65 C42 H42A 118.4 . . ? C72 C42 H42A 118.4 . . ? C51 C44 O2 119.5(7) . . ? C51 C44 C84 122.3(8) . . ? O2 C44 C84 118.0(7) . . ? C79 C46 C95 120.3(7) . . ? C79 C46 O12 118.5(7) . . ? C95 C46 O12 120.9(7) . . ? C69 C47 C68 120.0(7) . . ? C69 C47 O1 120.4(7) . . ? C68 C47 O1 119.5(7) . . ? C126 C48 C54 111.2(6) . . ? C126 C48 H48A 109.4 . . ? C54 C48 H48A 109.4 . . ? C126 C48 H48B 109.4 . . ? C54 C48 H48B 109.4 . . ? H48A C48 H48B 108.0 . . ? C127 C49 C173 119.6(8) . . ? C127 C49 H49A 120.2 . . ? C173 C49 H49A 120.2 . . ? C76 C50 C107 119.2(7) . . ? C76 C50 C94 121.7(8) . . ? C107 C50 C94 119.0(7) . . ? C44 C51 C138 118.3(7) . . ? C44 C51 C129 128.1(7) . . ? C138 C51 C129 113.6(7) . . ? C113 C52 C54 124.1(8) . . ? C113 C52 H52A 117.9 . . ? C54 C52 H52A 117.9 . . ? C76 C53 C59 117.7(7) . . ? C76 C53 C66 123.6(7) . . ? C59 C53 C66 118.6(7) . . ? C64 C54 C52 116.2(8) . . ? C64 C54 C48 123.3(7) . . ? C52 C54 C48 120.5(7) . . ? O7 C55 C86 124.2(8) . . ? O7 C55 C40 113.8(7) . . ? C86 C55 C40 122.0(8) . . ? C123 C56 C81 118.8(7) . . ? C123 C56 C101 119.5(7) . . ? C81 C56 C101 121.5(7) . . ? C115 C57 C155 118.8(7) . . ? C115 C57 H57A 120.6 . . ? C155 C57 H57A 120.6 . . ? C53 C59 C97 122.8(7) . . ? C53 C59 H59A 118.6 . . ? C97 C59 H59A 118.6 . . ? O11 C60 C102 120.3(8) . . ? O11 C60 C105 119.0(7) . . ? C102 C60 C105 120.7(8) . . ? C98 C61 C152 118.1(7) . . ? C98 C61 C85 120.0(7) . . ? C152 C61 C85 121.7(8) . . ? C92 C62 C145 118.1(8) . . ? C92 C62 H62A 121.0 . . ? C145 C62 H62A 121.0 . . ? C72 C63 C68 113.1(7) . . ? C72 C63 H63A 109.0 . . ? C68 C63 H63A 109.0 . . ? C72 C63 H63B 109.0 . . ? C68 C63 H63B 109.0 . . ? H63A C63 H63B 107.8 . . ? O14 C64 C54 122.4(8) . . ? O14 C64 C80 114.7(6) . . ? C54 C64 C80 122.9(7) . . ? C42 C65 C123 118.2(7) . . ? C42 C65 C83 122.1(7) . . ? C123 C65 C83 119.7(8) . . ? C109 C66 C53 111.0(6) . . ? C109 C66 H66A 109.4 . . ? C53 C66 H66A 109.4 . . ? C109 C66 H66B 109.5 . . ? C53 C66 H66B 109.4 . . ? H66A C66 H66B 108.0 . . ? C157 C67 C78 121.3(8) . . ? C157 C67 C130 126.6(8) . . ? C78 C67 C130 112.1(7) . . ? C145 C68 C47 118.4(7) . . ? C145 C68 C63 118.6(7) . . ? C47 C68 C63 122.5(7) . . ? C92 C69 C47 119.6(7) . . ? C92 C69 C129 113.8(7) . . ? C47 C69 C129 126.5(7) . . ? C75 C70 O3 118.7(7) . . ? C75 C70 C99 121.6(8) . . ? O3 C70 C99 119.7(7) . . ? C81 C72 C42 116.6(6) . . ? C81 C72 C63 123.6(7) . . ? C42 C72 C63 119.8(7) . . ? C84 C73 C86 110.8(7) . . ? C84 C73 H73A 109.5 . . ? C86 C73 H73A 109.5 . . ? C84 C73 H73B 109.5 . . ? C86 C73 H73B 109.5 . . ? H73A C73 H73B 108.1 . . ? C150 C74 C110 118.8(8) . . ? C150 C74 H74A 120.6 . . ? C110 C74 H74A 120.6 . . ? C70 C75 C93 120.4(8) . . ? C70 C75 C125 127.5(7) . . ? C93 C75 C125 112.1(7) . . ? C50 C76 O16 117.2(7) . . ? C50 C76 C53 121.6(8) . . ? O16 C76 C53 121.2(7) . . ? C134 C77 C155 118.8(8) . . ? C134 C77 C83 121.6(7) . . ? C155 C77 C83 119.6(8) . . ? C108 C78 C67 119.9(8) . . ? C108 C78 C137 126.0(8) . . ? C67 C78 C137 114.1(7) . . ? C46 C79 C150 119.0(8) . . ? C46 C79 C90 123.2(7) . . ? C150 C79 C90 117.7(7) . . ? C82 C80 C64 116.5(7) . . ? C82 C80 C120 123.8(8) . . ? C64 C80 C120 119.6(7) . . ? O6 C81 C56 117.1(7) . . ? O6 C81 C72 120.5(7) . . ? C56 C81 C72 122.4(7) . . ? C80 C82 C113 122.9(9) . . ? C80 C82 O13 115.4(7) . . ? C113 C82 O13 121.7(8) . . ? C77 C83 C65 113.4(7) . . ? C77 C83 H83A 108.9 . . ? C65 C83 H83A 108.9 . . ? C77 C83 H83B 108.9 . . ? C65 C83 H83B 108.9 . . ? H83A C83 H83B 107.7 . . ? C44 C84 C149 117.3(8) . . ? C44 C84 C73 123.0(8) . . ? C149 C84 C73 119.6(8) . . ? C61 C85 C99 112.4(6) . . ? C61 C85 H85A 109.1 . . ? C99 C85 H85A 109.1 . . ? C61 C85 H85B 109.1 . . ? C99 C85 H85B 109.1 . . ? H85A C85 H85B 107.8 . . ? C98 C86 C55 118.0(8) . . ? C98 C86 C73 120.5(7) . . ? C55 C86 C73 121.4(8) . . ? C118 C87 C162 120.3(8) . . ? C118 C87 H87A 119.8 . . ? C162 C87 H87A 119.8 . . ? C100 C88 C116 120.2(8) . . ? C100 C88 C137 126.0(8) . . ? C116 C88 C137 113.8(7) . . ? C40 C89 H89A 109.5 . . ? C40 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C40 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C79 C90 C113 111.2(6) . . ? C79 C90 H90A 109.4 . . ? C113 C90 H90A 109.4 . . ? C79 C90 H90B 109.4 . . ? C113 C90 H90B 109.4 . . ? H90A C90 H90B 108.0 . . ? C112 C91 C127 119.9(8) . . ? C112 C91 C137 126.9(8) . . ? C127 C91 C137 113.1(7) . . ? C62 C92 C69 121.0(8) . . ? C62 C92 C140 125.8(7) . . ? C69 C92 C140 113.2(7) . . ? C114 C93 C75 119.5(8) . . ? C114 C93 C143 127.0(8) . . ? C75 C93 C143 113.5(7) . . ? C50 C94 H94A 109.5 . . ? C50 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C50 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C110 C95 C46 120.4(8) . . ? C110 C95 C153 112.5(7) . . ? C46 C95 C153 127.0(7) . . ? C111 C96 C132 119.4(8) . . ? C111 C96 H96A 120.3 . . ? C132 C96 H96A 120.3 . . ? C107 C97 C59 115.9(8) . . ? C107 C97 C142 124.3(7) . . ? C59 C97 C142 119.7(7) . . ? C61 C98 C86 123.0(7) . . ? C61 C98 H98A 118.5 . . ? C86 C98 H98A 118.5 . . ? C70 C99 C124 117.6(7) . . ? C70 C99 C85 121.1(7) . . ? C124 C99 C85 121.0(7) . . ? C88 C100 O9 119.8(7) . . ? C88 C100 C109 121.3(8) . . ? O9 C100 C109 118.9(7) . . ? C56 C101 H10A 109.5 . . ? C56 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C56 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C118 C102 C60 120.8(8) . . ? C118 C102 C153 113.3(7) . . ? C60 C102 C153 125.7(8) . . ? C147 C103 C111 117.7(9) . . ? C147 C103 C143 129.2(8) . . ? C111 C103 C143 113.1(7) . . ? C121 C104 C159 120.0(9) . . ? C121 C104 H10D 120.0 . . ? C159 C104 H10D 120.0 . . ? C162 C105 C60 117.7(8) . . ? C162 C105 C142 120.9(7) . . ? C60 C105 C142 121.3(7) . . ? C161 C106 C135 121.9(9) . . ? C161 C106 C140 124.6(8) . . ? C135 C106 C140 113.5(7) . . ? O15 C107 C50 116.4(7) . . ? O15 C107 C97 120.9(7) . . ? C50 C107 C97 122.8(7) . . ? C78 C108 C141 118.0(9) . . ? C78 C108 H10E 121.0 . . ? C141 C108 H10E 121.0 . . ? C151 C109 C100 117.2(7) . . ? C151 C109 C66 121.8(8) . . ? C100 C109 C66 121.0(8) . . ? C95 C110 C74 120.6(8) . . ? C95 C110 C128 114.1(7) . . ? C74 C110 C128 125.1(8) . . ? C96 C111 C103 121.2(8) . . ? C96 C111 C125 126.8(8) . . ? C103 C111 C125 112.0(8) . . ? C91 C112 C126 120.9(8) . . ? C91 C112 O10 118.4(7) . . ? C126 C112 O10 120.7(7) . . ? C52 C113 C82 117.3(8) . . ? C52 C113 C90 121.8(7) . . ? C82 C113 C90 120.9(8) . . ? C93 C114 C124 119.8(8) . . ? C93 C114 H11A 120.1 . . ? C124 C114 H11A 120.1 . . ? C122 C115 C57 120.9(7) . . ? C122 C115 C143 112.5(7) . . ? C57 C115 C143 126.6(8) . . ? C117 C116 C88 119.7(7) . . ? C117 C116 C130 127.9(8) . . ? C88 C116 C130 112.4(7) . . ? C116 C117 C151 118.9(8) . . ? C116 C117 H11B 120.5 . . ? C151 C117 H11B 120.6 . . ? C87 C118 C102 119.6(8) . . ? C87 C118 C128 127.2(7) . . ? C102 C118 C128 113.2(7) . . ? C172 C119 C121 118.2(8) . . ? C172 C119 C128 127.8(7) . . ? C121 C119 C128 114.0(7) . . ? C80 C120 H12A 109.5 . . ? C80 C120 H12B 109.5 . . ? H12A C120 H12B 109.5 . . ? C80 C120 H12C 109.5 . . ? H12A C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? C104 C121 C119 121.0(8) . . ? C104 C121 C153 127.5(8) . . ? C119 C121 C153 111.4(7) . . ? C134 C122 C115 119.3(7) . . ? C134 C122 C125 126.6(7) . . ? C115 C122 C125 114.0(7) . . ? O5 C123 C56 115.4(7) . . ? O5 C123 C65 123.9(7) . . ? C56 C123 C65 120.8(8) . . ? C114 C124 C99 121.1(7) . . ? C114 C124 H12D 119.4 . . ? C99 C124 H12D 119.4 . . ? C122 C125 C75 105.7(6) . . ? C122 C125 C111 107.1(6) . . ? C75 C125 C111 104.4(6) . . ? C122 C125 H12E 113.0 . . ? C75 C125 H12E 113.0 . . ? C111 C125 H12E 113.0 . . ? C173 C126 C112 118.7(7) . . ? C173 C126 C48 121.0(7) . . ? C112 C126 C48 120.3(7) . . ? C49 C127 C91 119.3(8) . . ? C49 C127 C130 127.8(8) . . ? C91 C127 C130 112.9(7) . . ? C119 C128 C118 108.6(6) . . ? C119 C128 C110 103.9(7) . . ? C118 C128 C110 104.6(6) . . ? C119 C128 H12F 113.0 . . ? C118 C128 H12F 113.0 . . ? C110 C128 H12F 113.0 . . ? C135 C129 C51 106.5(6) . . ? C135 C129 C69 104.8(6) . . ? C51 C129 C69 104.3(6) . . ? C135 C129 H12G 113.4 . . ? C51 C129 H12G 113.4 . . ? C69 C129 H12G 113.4 . . ? C127 C130 C116 105.5(7) . . ? C127 C130 C67 106.4(7) . . ? C116 C130 C67 105.9(7) . . ? C127 C130 H13A 112.8 . . ? C116 C130 H13A 112.8 . . ? C67 C130 H13A 112.8 . . ? C138 C131 C149 119.3(8) . . ? C138 C131 H13B 120.4 . . ? C149 C131 H13B 120.4 . . ? C148 C132 C96 120.9(9) . . ? C148 C132 H13C 119.5 . . ? C96 C132 H13C 119.5 . . ? C122 C134 C77 121.4(7) . . ? C122 C134 O4 119.2(7) . . ? C77 C134 O4 119.3(7) . . ? C144 C135 C106 119.8(8) . . ? C144 C135 C129 126.2(8) . . ? C106 C135 C129 114.0(8) . . ? O11 C136 H13D 109.5 . . ? O11 C136 H13E 109.5 . . ? H13D C136 H13E 109.5 . . ? O11 C136 H13F 109.5 . . ? H13D C136 H13F 109.5 . . ? H13E C136 H13F 109.5 . . ? C78 C137 C88 104.0(6) . . ? C78 C137 C91 106.4(6) . . ? C88 C137 C91 105.6(6) . . ? C78 C137 H13G 113.4 . . ? C88 C137 H13G 113.4 . . ? C91 C137 H13G 113.4 . . ? C131 C138 C51 121.5(8) . . ? C131 C138 C140 125.9(8) . . ? C51 C138 C140 112.6(7) . . ? C159 C139 C172 121.4(8) . . ? C159 C139 H13H 119.3 . . ? C172 C139 H13H 119.3 . . ? C92 C140 C106 106.4(7) . . ? C92 C140 C138 103.5(7) . . ? C106 C140 C138 105.6(7) . . ? C92 C140 H14A 113.5 . . ? C106 C140 H14A 113.5 . . ? C138 C140 H14A 113.5 . . ? C166 C141 C108 120.8(9) . . ? C166 C141 H14B 119.6 . . ? C108 C141 H14B 119.6 . . ? C97 C142 C105 113.0(7) . . ? C97 C142 H14C 109.0 . . ? C105 C142 H14C 109.0 . . ? C97 C142 H14D 109.0 . . ? C105 C142 H14D 109.0 . . ? H14C C142 H14D 107.8 . . ? C103 C143 C93 105.4(7) . . ? C103 C143 C115 106.1(6) . . ? C93 C143 C115 106.3(6) . . ? C103 C143 H14E 112.8 . . ? C93 C143 H14E 112.8 . . ? C115 C143 H14E 112.8 . . ? C135 C144 C146 117.6(8) . . ? C135 C144 H14F 121.2 . . ? C146 C144 H14F 121.2 . . ? C68 C145 C62 122.8(8) . . ? C68 C145 H14G 118.6 . . ? C62 C145 H14G 118.6 . . ? C165 C146 C144 121.3(9) . . ? C165 C146 H14H 119.3 . . ? C144 C146 H14H 119.3 . . ? C103 C147 C148 120.8(9) . . ? C103 C147 H14I 119.6 . . ? C148 C147 H14I 119.6 . . ? C132 C148 C147 119.9(8) . . ? C132 C148 H14J 120.0 . . ? C147 C148 H14J 120.0 . . ? C131 C149 C84 121.2(8) . . ? C131 C149 H14K 119.4 . . ? C84 C149 H14K 119.4 . . ? C74 C150 C79 120.8(8) . . ? C74 C150 H15A 119.6 . . ? C79 C150 H15A 119.6 . . ? C109 C151 C117 122.6(8) . . ? C109 C151 H15B 118.7 . . ? C117 C151 H15B 118.7 . . ? O8 C152 C40 116.7(7) . . ? O8 C152 C61 121.3(8) . . ? C40 C152 C61 121.9(8) . . ? C95 C153 C121 105.3(6) . . ? C95 C153 C102 105.3(6) . . ? C121 C153 C102 105.9(7) . . ? C95 C153 H15C 113.2 . . ? C121 C153 H15C 113.2 . . ? C102 C153 H15C 113.2 . . ? O2 C154 H15D 109.5 . . ? O2 C154 H15E 109.5 . . ? H15D C154 H15E 109.5 . . ? O2 C154 H15F 109.5 . . ? H15D C154 H15F 109.5 . . ? H15E C154 H15F 109.5 . . ? C77 C155 C57 120.7(8) . . ? C77 C155 H15G 119.6 . . ? C57 C155 H15G 119.6 . . ? C67 C157 C166 119.1(8) . . ? C67 C157 H15H 120.4 . . ? C166 C157 H15H 120.4 . . ? C139 C159 C104 120.1(9) . . ? C139 C159 H15I 119.9 . . ? C104 C159 H15I 119.9 . . ? C106 C161 C165 119.0(9) . . ? C106 C161 H16A 120.5 . . ? C165 C161 H16A 120.5 . . ? C105 C162 C87 120.9(8) . . ? C105 C162 H16B 119.5 . . ? C87 C162 H16B 119.5 . . ? O10 C163 H16C 109.5 . . ? O10 C163 H16D 109.5 . . ? H16C C163 H16D 109.5 . . ? O10 C163 H16E 109.5 . . ? H16C C163 H16E 109.5 . . ? H16D C163 H16E 109.5 . . ? O3 C164 H16F 109.5 . . ? O3 C164 H16G 109.5 . . ? H16F C164 H16G 109.5 . . ? O3 C164 H16H 109.5 . . ? H16F C164 H16H 109.5 . . ? H16G C164 H16H 109.5 . . ? C146 C165 C161 120.4(9) . . ? C146 C165 H16I 119.8 . . ? C161 C165 H16I 119.8 . . ? C141 C166 C157 120.7(9) . . ? C141 C166 H16J 119.6 . . ? C157 C166 H16J 119.6 . . ? O1 C167 H16K 109.5 . . ? O1 C167 H16L 109.5 . . ? H16K C167 H16L 109.5 . . ? O1 C167 H16M 109.5 . . ? H16K C167 H16M 109.5 . . ? H16L C167 H16M 109.5 . . ? Cl12 C4A Cl10 111.5(6) . . ? Cl12 C4A Cl11 110.6(5) . . ? Cl10 C4A Cl11 110.0(5) . . ? Cl12 C4A H4AA 108.2 . . ? Cl10 C4A H4AA 108.2 . . ? Cl11 C4A H4AA 108.2 . . ? Cl4 C2A Cl6 111.5(7) . . ? Cl4 C2A Cl5 111.3(6) . . ? Cl6 C2A Cl5 110.6(6) . . ? Cl4 C2A H2AA 107.7 . . ? Cl6 C2A H2AA 107.7 . . ? Cl5 C2A H2AA 107.7 . . ? C139 C172 C119 119.3(8) . . ? C139 C172 H17A 120.4 . . ? C119 C172 H17A 120.4 . . ? C126 C173 C49 121.5(8) . . ? C126 C173 H17B 119.2 . . ? C49 C173 H17B 119.2 . . ? Cl16 C6A Cl17 114.5(7) . . ? Cl16 C6A Cl18 110.3(7) . . ? Cl17 C6A Cl18 110.3(6) . . ? Cl16 C6A H6AA 107.1 . . ? Cl17 C6A H6AA 107.1 . . ? Cl18 C6A H6AA 107.1 . . ? O12 C175 H17C 109.5 . . ? O12 C175 H17D 109.5 . . ? H17C C175 H17D 109.5 . . ? O12 C175 H17E 109.5 . . ? H17C C175 H17E 109.5 . . ? H17D C175 H17E 109.5 . . ? O4 C176 H17F 109.5 . . ? O4 C176 H17G 109.5 . . ? H17F C176 H17G 109.5 . . ? O4 C176 H17H 109.5 . . ? H17F C176 H17H 109.5 . . ? H17G C176 H17H 109.5 . . ? Cl2 C1A Cl1 112.3(6) . . ? Cl2 C1A Cl3 111.0(6) . . ? Cl1 C1A Cl3 111.6(7) . . ? Cl2 C1A H1AA 107.2 . . ? Cl1 C1A H1AA 107.2 . . ? Cl3 C1A H1AA 107.2 . . ? O9 C180 H18A 109.5 . . ? O9 C180 H18B 109.5 . . ? H18A C180 H18B 109.5 . . ? O9 C180 H18C 109.5 . . ? H18A C180 H18C 109.5 . . ? H18B C180 H18C 109.5 . . ? Cl7 C3A Cl9 122.9(8) . . ? Cl7 C3A Cl8 120.7(8) . . ? Cl9 C3A Cl8 116.4(8) . . ? Cl7 C3A H3A 90.0 . . ? Cl9 C3A H3A 90.0 . . ? Cl8 C3A H3A 90.0 . . ? Cl20 C7A Cl21 112.7(8) . . ? Cl20 C7A Cl19 111.7(9) . . ? Cl21 C7A Cl19 108.5(9) . . ? Cl20 C7A H7AA 107.9 . . ? Cl21 C7A H7AA 107.9 . . ? Cl19 C7A H7AA 107.9 . . ? Cl13 C5A Cl15 120.8(10) . . ? Cl13 C5A Cl14 119.7(10) . . ? Cl15 C5A Cl14 118.2(8) . . ? Cl13 C5A H5A 93.8 . . ? Cl15 C5A H5A 93.8 . . ? Cl14 C5A H5A 93.8 . . ? Cl23 C8A Cl22 112.1(10) . . ? Cl23 C8A Cl24 110.9(8) . . ? Cl22 C8A Cl24 110.6(8) . . ? Cl23 C8A H8AA 107.7 . . ? Cl22 C8A H8AA 107.7 . . ? Cl24 C8A H8AA 107.7 . . ? Cl25 C9A Cl26 112.7(9) . . ? Cl25 C9A Cl27 111.4(8) . . ? Cl26 C9A Cl27 110.2(9) . . ? Cl25 C9A H9AA 107.4 . . ? Cl26 C9A H9AA 107.4 . . ? Cl27 C9A H9AA 107.4 . . ? Cl30 C10A Cl28 118.9(9) . . ? Cl30 C10A Cl29 92.7(11) . . ? Cl28 C10A Cl29 91.7(16) . . ? Cl30 C10A H10F 116.0 . . ? Cl28 C10A H10F 116.0 . . ? Cl29 C10A H10F 116.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C154 O2 C44 C51 92.6(9) . . . . ? C154 O2 C44 C84 -91.7(9) . . . . ? C175 O12 C46 C79 -103.3(8) . . . . ? C175 O12 C46 C95 82.6(9) . . . . ? C167 O1 C47 C69 -81.8(9) . . . . ? C167 O1 C47 C68 102.3(8) . . . . ? O2 C44 C51 C138 179.9(7) . . . . ? C84 C44 C51 C138 4.3(13) . . . . ? O2 C44 C51 C129 0.4(13) . . . . ? C84 C44 C51 C129 -175.2(8) . . . . ? C113 C52 C54 C64 0.8(11) . . . . ? C113 C52 C54 C48 -178.5(7) . . . . ? C126 C48 C54 C64 -88.8(9) . . . . ? C126 C48 C54 C52 90.5(8) . . . . ? C152 C40 C55 O7 -176.1(7) . . . . ? C89 C40 C55 O7 -3.2(11) . . . . ? C152 C40 C55 C86 4.9(11) . . . . ? C89 C40 C55 C86 177.8(7) . . . . ? C76 C53 C59 C97 -1.4(11) . . . . ? C66 C53 C59 C97 175.3(7) . . . . ? C136 O11 C60 C102 -89.8(9) . . . . ? C136 O11 C60 C105 92.5(9) . . . . ? C52 C54 C64 O14 179.5(7) . . . . ? C48 C54 C64 O14 -1.2(12) . . . . ? C52 C54 C64 C80 0.5(11) . . . . ? C48 C54 C64 C80 179.8(7) . . . . ? C72 C42 C65 C123 -0.9(12) . . . . ? C72 C42 C65 C83 178.2(7) . . . . ? C76 C53 C66 C109 87.3(9) . . . . ? C59 C53 C66 C109 -89.1(9) . . . . ? C69 C47 C68 C145 -1.4(12) . . . . ? O1 C47 C68 C145 174.5(7) . . . . ? C69 C47 C68 C63 -172.8(7) . . . . ? O1 C47 C68 C63 3.2(11) . . . . ? C72 C63 C68 C145 -81.7(9) . . . . ? C72 C63 C68 C47 89.6(10) . . . . ? C68 C47 C69 C92 -0.3(12) . . . . ? O1 C47 C69 C92 -176.2(7) . . . . ? C68 C47 C69 C129 177.6(7) . . . . ? O1 C47 C69 C129 1.7(12) . . . . ? C164 O3 C70 C75 -80.3(9) . . . . ? C164 O3 C70 C99 101.8(9) . . . . ? C65 C42 C72 C81 1.1(11) . . . . ? C65 C42 C72 C63 -177.5(7) . . . . ? C68 C63 C72 C81 -89.9(9) . . . . ? C68 C63 C72 C42 88.6(9) . . . . ? O3 C70 C75 C93 180.0(7) . . . . ? C99 C70 C75 C93 -2.1(13) . . . . ? O3 C70 C75 C125 1.2(13) . . . . ? C99 C70 C75 C125 179.1(8) . . . . ? C107 C50 C76 O16 -179.6(7) . . . . ? C94 C50 C76 O16 -1.1(11) . . . . ? C107 C50 C76 C53 -0.6(11) . . . . ? C94 C50 C76 C53 178.0(7) . . . . ? C59 C53 C76 C50 2.1(11) . . . . ? C66 C53 C76 C50 -174.3(7) . . . . ? C59 C53 C76 O16 -178.9(6) . . . . ? C66 C53 C76 O16 4.7(11) . . . . ? C157 C67 C78 C108 4.7(12) . . . . ? C130 C67 C78 C108 -175.6(7) . . . . ? C157 C67 C78 C137 -176.7(7) . . . . ? C130 C67 C78 C137 3.0(9) . . . . ? C95 C46 C79 C150 -0.8(12) . . . . ? O12 C46 C79 C150 -174.9(7) . . . . ? C95 C46 C79 C90 175.7(7) . . . . ? O12 C46 C79 C90 1.6(12) . . . . ? O14 C64 C80 C82 -179.3(7) . . . . ? C54 C64 C80 C82 -0.3(12) . . . . ? O14 C64 C80 C120 4.7(11) . . . . ? C54 C64 C80 C120 -176.2(8) . . . . ? C123 C56 C81 O6 -180.0(7) . . . . ? C101 C56 C81 O6 5.3(11) . . . . ? C123 C56 C81 C72 -1.9(12) . . . . ? C101 C56 C81 C72 -176.7(7) . . . . ? C42 C72 C81 O6 178.3(7) . . . . ? C63 C72 C81 O6 -3.2(11) . . . . ? C42 C72 C81 C56 0.3(11) . . . . ? C63 C72 C81 C56 178.8(7) . . . . ? C64 C80 C82 C113 -1.3(12) . . . . ? C120 C80 C82 C113 174.4(8) . . . . ? C64 C80 C82 O13 -179.5(7) . . . . ? C120 C80 C82 O13 -3.7(12) . . . . ? C134 C77 C83 C65 -91.3(10) . . . . ? C155 C77 C83 C65 87.4(9) . . . . ? C42 C65 C83 C77 -91.0(9) . . . . ? C123 C65 C83 C77 88.1(9) . . . . ? C51 C44 C84 C149 -2.9(13) . . . . ? O2 C44 C84 C149 -178.5(7) . . . . ? C51 C44 C84 C73 176.5(8) . . . . ? O2 C44 C84 C73 0.9(12) . . . . ? C86 C73 C84 C44 -96.6(10) . . . . ? C86 C73 C84 C149 82.8(9) . . . . ? C98 C61 C85 C99 87.5(9) . . . . ? C152 C61 C85 C99 -87.2(9) . . . . ? O7 C55 C86 C98 179.1(7) . . . . ? C40 C55 C86 C98 -2.1(11) . . . . ? O7 C55 C86 C73 -0.2(12) . . . . ? C40 C55 C86 C73 178.6(7) . . . . ? C84 C73 C86 C98 -95.0(9) . . . . ? C84 C73 C86 C55 84.2(9) . . . . ? C46 C79 C90 C113 -94.7(9) . . . . ? C150 C79 C90 C113 81.8(9) . . . . ? C145 C62 C92 C69 0.7(12) . . . . ? C145 C62 C92 C140 -177.6(8) . . . . ? C47 C69 C92 C62 0.7(13) . . . . ? C129 C69 C92 C62 -177.5(7) . . . . ? C47 C69 C92 C140 179.1(7) . . . . ? C129 C69 C92 C140 1.0(10) . . . . ? C70 C75 C93 C114 2.2(12) . . . . ? C125 C75 C93 C114 -178.9(7) . . . . ? C70 C75 C93 C143 -178.7(7) . . . . ? C125 C75 C93 C143 0.3(9) . . . . ? C79 C46 C95 C110 3.3(12) . . . . ? O12 C46 C95 C110 177.2(7) . . . . ? C79 C46 C95 C153 -177.4(7) . . . . ? O12 C46 C95 C153 -3.4(12) . . . . ? C53 C59 C97 C107 -0.8(11) . . . . ? C53 C59 C97 C142 -177.6(7) . . . . ? C152 C61 C98 C86 1.3(12) . . . . ? C85 C61 C98 C86 -173.5(7) . . . . ? C55 C86 C98 C61 -1.2(12) . . . . ? C73 C86 C98 C61 178.1(7) . . . . ? C75 C70 C99 C124 0.2(12) . . . . ? O3 C70 C99 C124 178.1(7) . . . . ? C75 C70 C99 C85 -173.7(8) . . . . ? O3 C70 C99 C85 4.1(12) . . . . ? C61 C85 C99 C70 89.7(10) . . . . ? C61 C85 C99 C124 -84.0(9) . . . . ? C116 C88 C100 O9 -178.4(7) . . . . ? C137 C88 C100 O9 -0.8(12) . . . . ? C116 C88 C100 C109 5.2(12) . . . . ? C137 C88 C100 C109 -177.2(7) . . . . ? C180 O9 C100 C88 80.7(9) . . . . ? C180 O9 C100 C109 -102.8(8) . . . . ? O11 C60 C102 C118 -177.9(7) . . . . ? C105 C60 C102 C118 -0.3(12) . . . . ? O11 C60 C102 C153 -3.5(13) . . . . ? C105 C60 C102 C153 174.2(8) . . . . ? O11 C60 C105 C162 178.5(7) . . . . ? C102 C60 C105 C162 0.8(12) . . . . ? O11 C60 C105 C142 2.6(12) . . . . ? C102 C60 C105 C142 -175.1(7) . . . . ? C76 C50 C107 O15 178.1(7) . . . . ? C94 C50 C107 O15 -0.5(10) . . . . ? C76 C50 C107 C97 -1.9(11) . . . . ? C94 C50 C107 C97 179.5(7) . . . . ? C59 C97 C107 O15 -177.4(6) . . . . ? C142 C97 C107 O15 -0.8(12) . . . . ? C59 C97 C107 C50 2.5(11) . . . . ? C142 C97 C107 C50 179.1(7) . . . . ? C67 C78 C108 C141 -2.2(11) . . . . ? C137 C78 C108 C141 179.5(7) . . . . ? C88 C100 C109 C151 -3.8(12) . . . . ? O9 C100 C109 C151 179.8(7) . . . . ? C88 C100 C109 C66 175.7(7) . . . . ? O9 C100 C109 C66 -0.8(11) . . . . ? C53 C66 C109 C151 88.0(9) . . . . ? C53 C66 C109 C100 -91.4(9) . . . . ? C46 C95 C110 C74 -4.7(12) . . . . ? C153 C95 C110 C74 175.9(7) . . . . ? C46 C95 C110 C128 -179.6(7) . . . . ? C153 C95 C110 C128 0.9(10) . . . . ? C150 C74 C110 C95 3.5(12) . . . . ? C150 C74 C110 C128 177.9(8) . . . . ? C132 C96 C111 C103 1.0(12) . . . . ? C132 C96 C111 C125 179.4(8) . . . . ? C147 C103 C111 C96 -2.0(12) . . . . ? C143 C103 C111 C96 176.1(7) . . . . ? C147 C103 C111 C125 179.3(7) . . . . ? C143 C103 C111 C125 -2.5(9) . . . . ? C127 C91 C112 C126 -0.8(12) . . . . ? C137 C91 C112 C126 175.4(8) . . . . ? C127 C91 C112 O10 -178.4(7) . . . . ? C137 C91 C112 O10 -2.2(13) . . . . ? C163 O10 C112 C91 -92.9(9) . . . . ? C163 O10 C112 C126 89.5(9) . . . . ? C54 C52 C113 C82 -2.3(12) . . . . ? C54 C52 C113 C90 177.6(7) . . . . ? C80 C82 C113 C52 2.5(12) . . . . ? O13 C82 C113 C52 -179.4(7) . . . . ? C80 C82 C113 C90 -177.4(7) . . . . ? O13 C82 C113 C90 0.7(11) . . . . ? C79 C90 C113 C52 -89.0(9) . . . . ? C79 C90 C113 C82 90.9(9) . . . . ? C75 C93 C114 C124 -0.3(13) . . . . ? C143 C93 C114 C124 -179.4(8) . . . . ? C155 C57 C115 C122 -1.7(12) . . . . ? C155 C57 C115 C143 175.6(8) . . . . ? C100 C88 C116 C117 -3.9(13) . . . . ? C137 C88 C116 C117 178.2(8) . . . . ? C100 C88 C116 C130 177.3(7) . . . . ? C137 C88 C116 C130 -0.6(10) . . . . ? C88 C116 C117 C151 1.4(13) . . . . ? C130 C116 C117 C151 -179.9(8) . . . . ? C162 C87 C118 C102 1.5(13) . . . . ? C162 C87 C118 C128 -177.4(8) . . . . ? C60 C102 C118 C87 -0.9(12) . . . . ? C153 C102 C118 C87 -176.0(7) . . . . ? C60 C102 C118 C128 178.1(7) . . . . ? C153 C102 C118 C128 3.0(10) . . . . ? C159 C104 C121 C119 -1.4(13) . . . . ? C159 C104 C121 C153 -177.8(8) . . . . ? C172 C119 C121 C104 2.6(12) . . . . ? C128 C119 C121 C104 -178.6(7) . . . . ? C172 C119 C121 C153 179.6(7) . . . . ? C128 C119 C121 C153 -1.6(10) . . . . ? C57 C115 C122 C134 0.6(12) . . . . ? C143 C115 C122 C134 -177.1(7) . . . . ? C57 C115 C122 C125 178.8(7) . . . . ? C143 C115 C122 C125 1.1(10) . . . . ? C81 C56 C123 O5 -179.2(7) . . . . ? C101 C56 C123 O5 -4.3(11) . . . . ? C81 C56 C123 C65 2.2(12) . . . . ? C101 C56 C123 C65 177.0(7) . . . . ? C42 C65 C123 O5 -179.4(7) . . . . ? C83 C65 C123 O5 1.5(11) . . . . ? C42 C65 C123 C56 -0.8(12) . . . . ? C83 C65 C123 C56 -179.9(7) . . . . ? C93 C114 C124 C99 -1.6(13) . . . . ? C70 C99 C124 C114 1.7(12) . . . . ? C85 C99 C124 C114 175.6(8) . . . . ? C134 C122 C125 C75 121.4(9) . . . . ? C115 C122 C125 C75 -56.6(9) . . . . ? C134 C122 C125 C111 -127.7(8) . . . . ? C115 C122 C125 C111 54.3(9) . . . . ? C70 C75 C125 C122 -126.0(9) . . . . ? C93 C75 C125 C122 55.2(8) . . . . ? C70 C75 C125 C111 121.2(9) . . . . ? C93 C75 C125 C111 -57.7(8) . . . . ? C96 C111 C125 C122 128.6(8) . . . . ? C103 C111 C125 C122 -52.9(8) . . . . ? C96 C111 C125 C75 -119.6(9) . . . . ? C103 C111 C125 C75 58.9(8) . . . . ? C91 C112 C126 C173 2.7(12) . . . . ? O10 C112 C126 C173 -179.7(7) . . . . ? C91 C112 C126 C48 -177.0(7) . . . . ? O10 C112 C126 C48 0.6(12) . . . . ? C54 C48 C126 C173 -90.2(9) . . . . ? C54 C48 C126 C112 89.5(9) . . . . ? C173 C49 C127 C91 2.3(13) . . . . ? C173 C49 C127 C130 -178.1(8) . . . . ? C112 C91 C127 C49 -1.8(12) . . . . ? C137 C91 C127 C49 -178.5(8) . . . . ? C112 C91 C127 C130 178.5(7) . . . . ? C137 C91 C127 C130 1.9(10) . . . . ? C172 C119 C128 C118 125.2(9) . . . . ? C121 C119 C128 C118 -53.5(9) . . . . ? C172 C119 C128 C110 -124.0(9) . . . . ? C121 C119 C128 C110 57.4(9) . . . . ? C87 C118 C128 C119 -128.3(9) . . . . ? C102 C118 C128 C119 52.7(9) . . . . ? C87 C118 C128 C110 121.3(9) . . . . ? C102 C118 C128 C110 -57.7(9) . . . . ? C95 C110 C128 C119 -57.8(9) . . . . ? C74 C110 C128 C119 127.6(8) . . . . ? C95 C110 C128 C118 56.0(9) . . . . ? C74 C110 C128 C118 -118.7(8) . . . . ? C44 C51 C129 C135 -124.8(9) . . . . ? C138 C51 C129 C135 55.7(9) . . . . ? C44 C51 C129 C69 124.6(9) . . . . ? C138 C51 C129 C69 -54.8(9) . . . . ? C92 C69 C129 C135 -55.8(9) . . . . ? C47 C69 C129 C135 126.2(9) . . . . ? C92 C69 C129 C51 56.0(9) . . . . ? C47 C69 C129 C51 -122.0(9) . . . . ? C49 C127 C130 C116 122.6(9) . . . . ? C91 C127 C130 C116 -57.8(9) . . . . ? C49 C127 C130 C67 -125.2(9) . . . . ? C91 C127 C130 C67 54.4(9) . . . . ? C117 C116 C130 C127 -121.5(10) . . . . ? C88 C116 C130 C127 57.2(9) . . . . ? C117 C116 C130 C67 125.9(9) . . . . ? C88 C116 C130 C67 -55.4(9) . . . . ? C157 C67 C130 C127 122.1(8) . . . . ? C78 C67 C130 C127 -57.6(8) . . . . ? C157 C67 C130 C116 -126.0(8) . . . . ? C78 C67 C130 C116 54.3(9) . . . . ? C111 C96 C132 C148 1.8(13) . . . . ? C115 C122 C134 C77 1.7(12) . . . . ? C125 C122 C134 C77 -176.3(7) . . . . ? C115 C122 C134 O4 178.3(7) . . . . ? C125 C122 C134 O4 0.3(12) . . . . ? C155 C77 C134 C122 -2.7(12) . . . . ? C83 C77 C134 C122 175.9(7) . . . . ? C155 C77 C134 O4 -179.3(7) . . . . ? C83 C77 C134 O4 -0.7(11) . . . . ? C176 O4 C134 C122 91.3(9) . . . . ? C176 O4 C134 C77 -92.0(9) . . . . ? C161 C106 C135 C144 0.8(12) . . . . ? C140 C106 C135 C144 178.0(7) . . . . ? C161 C106 C135 C129 -179.3(8) . . . . ? C140 C106 C135 C129 -2.1(10) . . . . ? C51 C129 C135 C144 125.8(9) . . . . ? C69 C129 C135 C144 -124.0(9) . . . . ? C51 C129 C135 C106 -54.1(9) . . . . ? C69 C129 C135 C106 56.1(9) . . . . ? C108 C78 C137 C88 120.3(8) . . . . ? C67 C78 C137 C88 -58.2(8) . . . . ? C108 C78 C137 C91 -128.5(8) . . . . ? C67 C78 C137 C91 53.0(8) . . . . ? C100 C88 C137 C78 -120.7(8) . . . . ? C116 C88 C137 C78 57.1(9) . . . . ? C100 C88 C137 C91 127.5(8) . . . . ? C116 C88 C137 C91 -54.7(9) . . . . ? C112 C91 C137 C78 127.5(9) . . . . ? C127 C91 C137 C78 -56.1(9) . . . . ? C112 C91 C137 C88 -122.4(9) . . . . ? C127 C91 C137 C88 54.0(9) . . . . ? C149 C131 C138 C51 -0.5(13) . . . . ? C149 C131 C138 C140 177.7(8) . . . . ? C44 C51 C138 C131 -2.5(13) . . . . ? C129 C51 C138 C131 177.0(8) . . . . ? C44 C51 C138 C140 179.0(7) . . . . ? C129 C51 C138 C140 -1.5(10) . . . . ? C62 C92 C140 C106 -128.1(9) . . . . ? C69 C92 C140 C106 53.6(9) . . . . ? C62 C92 C140 C138 120.9(9) . . . . ? C69 C92 C140 C138 -57.4(9) . . . . ? C161 C106 C140 C92 123.5(8) . . . . ? C135 C106 C140 C92 -53.6(9) . . . . ? C161 C106 C140 C138 -126.9(9) . . . . ? C135 C106 C140 C138 56.0(9) . . . . ? C131 C138 C140 C92 -120.3(9) . . . . ? C51 C138 C140 C92 58.1(9) . . . . ? C131 C138 C140 C106 128.1(9) . . . . ? C51 C138 C140 C106 -53.5(9) . . . . ? C78 C108 C141 C166 -1.1(13) . . . . ? C107 C97 C142 C105 -85.6(9) . . . . ? C59 C97 C142 C105 90.8(9) . . . . ? C162 C105 C142 C97 -82.7(9) . . . . ? C60 C105 C142 C97 93.1(9) . . . . ? C147 C103 C143 C93 122.9(9) . . . . ? C111 C103 C143 C93 -55.0(8) . . . . ? C147 C103 C143 C115 -124.6(9) . . . . ? C111 C103 C143 C115 57.6(9) . . . . ? C114 C93 C143 C103 -124.4(9) . . . . ? C75 C93 C143 C103 56.5(8) . . . . ? C114 C93 C143 C115 123.2(9) . . . . ? C75 C93 C143 C115 -55.8(9) . . . . ? C122 C115 C143 C103 -56.9(9) . . . . ? C57 C115 C143 C103 125.6(9) . . . . ? C122 C115 C143 C93 55.0(9) . . . . ? C57 C115 C143 C93 -122.5(9) . . . . ? C106 C135 C144 C146 -0.6(12) . . . . ? C129 C135 C144 C146 179.5(8) . . . . ? C47 C68 C145 C62 2.9(13) . . . . ? C63 C68 C145 C62 174.6(8) . . . . ? C92 C62 C145 C68 -2.5(13) . . . . ? C135 C144 C146 C165 0.6(13) . . . . ? C111 C103 C147 C148 0.3(12) . . . . ? C143 C103 C147 C148 -177.5(8) . . . . ? C96 C132 C148 C147 -3.5(13) . . . . ? C103 C147 C148 C132 2.5(13) . . . . ? C138 C131 C149 C84 2.0(13) . . . . ? C44 C84 C149 C131 -0.3(13) . . . . ? C73 C84 C149 C131 -179.8(8) . . . . ? C110 C74 C150 C79 -1.0(13) . . . . ? C46 C79 C150 C74 -0.3(13) . . . . ? C90 C79 C150 C74 -177.0(8) . . . . ? C100 C109 C151 C117 1.3(13) . . . . ? C66 C109 C151 C117 -178.2(8) . . . . ? C116 C117 C151 C109 -0.2(13) . . . . ? C55 C40 C152 O8 178.8(7) . . . . ? C89 C40 C152 O8 5.8(11) . . . . ? C55 C40 C152 C61 -4.8(11) . . . . ? C89 C40 C152 C61 -177.8(7) . . . . ? C98 C61 C152 O8 178.0(7) . . . . ? C85 C61 C152 O8 -7.3(11) . . . . ? C98 C61 C152 C40 1.8(11) . . . . ? C85 C61 C152 C40 176.5(7) . . . . ? C110 C95 C153 C121 55.9(8) . . . . ? C46 C95 C153 C121 -123.5(8) . . . . ? C110 C95 C153 C102 -55.7(9) . . . . ? C46 C95 C153 C102 124.9(8) . . . . ? C104 C121 C153 C95 121.2(9) . . . . ? C119 C121 C153 C95 -55.6(8) . . . . ? C104 C121 C153 C102 -127.6(9) . . . . ? C119 C121 C153 C102 55.7(9) . . . . ? C118 C102 C153 C95 54.1(9) . . . . ? C60 C102 C153 C95 -120.8(8) . . . . ? C118 C102 C153 C121 -57.2(9) . . . . ? C60 C102 C153 C121 128.0(8) . . . . ? C134 C77 C155 C57 1.6(12) . . . . ? C83 C77 C155 C57 -177.1(7) . . . . ? C115 C57 C155 C77 0.6(12) . . . . ? C78 C67 C157 C166 -3.8(12) . . . . ? C130 C67 C157 C166 176.5(8) . . . . ? C172 C139 C159 C104 -1.3(15) . . . . ? C121 C104 C159 C139 0.7(14) . . . . ? C135 C106 C161 C165 -1.0(13) . . . . ? C140 C106 C161 C165 -177.9(8) . . . . ? C60 C105 C162 C87 -0.2(12) . . . . ? C142 C105 C162 C87 175.7(8) . . . . ? C118 C87 C162 C105 -1.0(13) . . . . ? C144 C146 C165 C161 -0.9(15) . . . . ? C106 C161 C165 C146 1.1(14) . . . . ? C108 C141 C166 C157 2.0(14) . . . . ? C67 C157 C166 C141 0.5(13) . . . . ? C159 C139 C172 C119 2.6(14) . . . . ? C121 C119 C172 C139 -3.2(12) . . . . ? C128 C119 C172 C139 178.2(8) . . . . ? C112 C126 C173 C49 -2.2(13) . . . . ? C48 C126 C173 C49 177.5(8) . . . . ? C127 C49 C173 C126 -0.3(13) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.372 _refine_diff_density_min -0.987 _refine_diff_density_rms 0.120 _database_code_depnum_ccdc_archive 'CCDC 931783'